CN114474482A - A kind of preparation technology of bioceramic-degradable polymer composite granulation - Google Patents
A kind of preparation technology of bioceramic-degradable polymer composite granulation Download PDFInfo
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Abstract
本发明公开了一种生物陶瓷‑可降解高分子复合造粒的制备工艺,包括:将生物陶瓷粉末与可降解高分子材料粉末按比例混合后,放入球磨机,使用大、中、小磨球进行机械球磨,得到复合粉末,将复合粉末放入真空系统进行真空干燥;将复合粉末投入至挤出机中,启动水冷拉条切粒系统、水循环系统、吹干机和切粒机,物料经挤出机基础,冷却成型,切割成粒,得到生物陶瓷‑可降解高分子复合材料。本发明结合机械球磨与挤出造粒工艺的优势,利用机械球磨工艺强大的冲击力、剪切力和碾压力,实现陶瓷和高分子均匀混合;利用挤出造粒工艺优异的熔融、挤出、混合能力,实现陶瓷和高分子的塑化、包裹、造粒,制备出一种满足再生组织器官要求的复合材料。
The invention discloses a preparation process of bioceramic-degradable polymer composite granulation, comprising: mixing bioceramic powder and degradable polymer material powder in proportion, putting them into a ball mill, and using large, medium and small grinding balls Perform mechanical ball milling to obtain composite powder, put the composite powder into the vacuum system for vacuum drying; put the composite powder into the extruder, start the water-cooled strand pelletizing system, water circulation system, blow dryer and pelletizer. Extruder basis, cooling molding, cutting into granules to obtain bioceramic-degradable polymer composite materials. The invention combines the advantages of mechanical ball milling and extrusion granulation technology, and utilizes the strong impact force, shear force and rolling force of the mechanical ball milling process to achieve uniform mixing of ceramics and polymers; It can realize the plasticization, packaging and granulation of ceramics and polymers, and prepare a composite material that meets the requirements of regenerating tissues and organs.
Description
技术领域technical field
本发明属于生物材料制备技术领域,更具体地说,本发明涉及一种生物陶瓷-可降解高分子复合造粒的制备工艺。The invention belongs to the technical field of biological material preparation, and more particularly, the invention relates to a preparation process of bioceramic-degradable polymer composite granulation.
背景技术Background technique
生物陶瓷由于在组成、结构上与人体硬组织的无机成份相似而具有良好的生物相容性、生物活性和组织传导性,但存在韧性差、脆性大、降解速率慢等问题;生物可降解高分子材料具有良好的生物相容性、生物降解性、无毒,且力学相容性和成型性较好,是组织再生与修复中选用最多的支架材料,但不足之处在于其机械强度较差,不具有生物活性和组织传导性。因此,单一的生物陶瓷或生物可降解高分子材料都不是理想的组织修复与再生材料。通过将两种或多种材料复合在一起,能实现性能互补,使材料的性能更优。Bioceramics have good biocompatibility, bioactivity and tissue conductivity due to their similarity in composition and structure to the inorganic components of human hard tissues, but they have problems such as poor toughness, high brittleness, and slow degradation rate; high biodegradability Molecular materials have good biocompatibility, biodegradability, non-toxicity, and good mechanical compatibility and formability. They are the most used scaffold materials in tissue regeneration and repair, but the disadvantage is that their mechanical strength is poor. , does not have biological activity and tissue conductivity. Therefore, a single bioceramic or biodegradable polymer material is not an ideal tissue repair and regeneration material. By compounding two or more materials together, complementary properties can be achieved and the properties of the materials are better.
生物陶瓷颗粒在可降解高分子材料中均匀分散是决定其复合材料性能的关键。目前,常用的分散方式主要有超声分散、机械搅拌、机械球磨等。其中,机械球磨能通过施加不连续的高应变率,对粉体反复地冲击、研磨、剪切,改变粉末的尺寸、特征长度、形态等,使粉末产生塑性变形、断裂、细化团聚粉末,从而促进陶瓷颗粒在高分子材料中均匀分散。此外,球磨过程会产生机械驱动力与热力学驱动力,两者力的结合可以诱导固体中化学物质强迫混合,从而增强陶瓷与高分子共混物在原子尺度上的均匀性。The uniform dispersion of bioceramic particles in degradable polymer materials is the key to determine the properties of their composites. At present, the commonly used dispersion methods mainly include ultrasonic dispersion, mechanical stirring, and mechanical ball milling. Among them, mechanical ball milling can repeatedly impact, grind, and shear the powder by applying a discontinuous high strain rate, changing the size, characteristic length, shape, etc. of the powder, so as to cause the powder to plastically deform, fracture, and refine the agglomerated powder. So as to promote the uniform dispersion of ceramic particles in the polymer material. In addition, the ball milling process will generate mechanical driving force and thermodynamic driving force, and the combination of the two forces can induce the forced mixing of chemical substances in the solid, thereby enhancing the uniformity of ceramic and polymer blends at the atomic scale.
需要指出的是,机械球磨后的复合粉体只是通过简单的机械嵌入、表面吸附、物理接触等方式结合,结合力较弱,在运输、储存、流通加工与装卸搬运等过程中由于密度间的差异会重新出现分层。挤出造粒工艺作为一种热塑复合工艺,能够在挤出过程中产生塑性耗散热、黏性耗散热和粉末间相互摩擦热,促进复合粉体的熔融、混合及分散;同时,该工艺的螺杆旋转能产生强大的挤压力、拉伸力与剪切力,使复合粉体发生塑性变形,实现复合粉体塑化、包裹、造粒,从而维持陶瓷在高分子材料基体中的均匀分散。It should be pointed out that the composite powder after mechanical ball milling is only combined by simple mechanical embedding, surface adsorption, physical contact, etc., and the binding force is weak. Differences reappear stratified. As a thermoplastic composite process, extrusion granulation process can generate plastic heat dissipation, viscous heat dissipation and mutual friction heat between powders in the extrusion process, and promote the melting, mixing and dispersion of composite powders; at the same time, this process The rotation of the screw can generate strong extrusion force, tensile force and shear force, which can cause the composite powder to plastically deform, realize the plasticization, wrapping and granulation of the composite powder, so as to maintain the uniformity of the ceramic in the polymer material matrix. dispersion.
发明内容SUMMARY OF THE INVENTION
本发明的一个目的是解决至少上述问题和/或缺陷,并提供至少后面将说明的优点。SUMMARY OF THE INVENTION An object of the present invention is to address at least the above-mentioned problems and/or disadvantages and to provide at least the advantages that will be described hereinafter.
为了实现根据本发明的这些目的和其它优点,提供了一种生物陶瓷-客家凝结高分子复合造粒的制备工艺,包括:In order to achieve these objects and other advantages according to the present invention, a preparation process of bioceramic-Hakka coagulation polymer composite granulation is provided, comprising:
优选的是,其中,包括机械球磨与挤出造粒工艺,其中所述机械球磨工艺包括:将生物陶瓷粉末与可降解高分子材料粉末按比例混合后,放入球磨机,使用大、中、小磨球进行机械球磨,得到复合粉末,将复合粉末放入真空系统进行真空干燥;Preferably, the process includes mechanical ball milling and extrusion granulation, wherein the mechanical ball milling process includes: after mixing the bioceramic powder and the degradable polymer material powder in proportion, put it into a ball mill, and use large, medium and small The grinding ball is subjected to mechanical ball milling to obtain composite powder, and the composite powder is put into a vacuum system for vacuum drying;
机械球磨后进行挤出造粒工艺,所述挤出造粒工艺包括:设置挤出机各区的温度,设置余热时间及温度,设置螺杆转速、物料停留时间、熔体压力,启动喂料电机,将复合粉末投入至挤出机中,启动水冷拉条切粒系统、水循环系统、吹干机和切粒机,物料经挤出机基础,冷却成型,切割成粒,得到生物陶瓷-可降解高分子复合材料。The extrusion granulation process is carried out after the mechanical ball milling. The extrusion granulation process includes: setting the temperature of each zone of the extruder, setting the residual heat time and temperature, setting the screw speed, material residence time, melt pressure, starting the feeding motor, Put the composite powder into the extruder, start the water-cooled strand pelletizing system, the water circulation system, the dryer and the pelletizer. Molecular composites.
优选的是,其中,所述机械球磨工艺中,大、中、小磨球的质量比为1∶1∶1~1∶5∶7;Preferably, wherein, in the mechanical ball milling process, the mass ratio of large, medium and small grinding balls is 1:1:1 to 1:5:7;
所述大、中、小磨球均为氧化锆球,其中,大、中、小氧化锆球的直径范围分别为3~4cm,1~3cm,0~1cm;大、中、小磨球与生物陶瓷粉末、可降解高分子材料粉末总质量的重量比为1∶1~1∶20。The large, medium and small grinding balls are all zirconia balls, wherein the diameter ranges of the large, medium and small zirconia balls are 3-4 cm, 1-3 cm and 0-1 cm respectively; The weight ratio of the total mass of the bioceramic powder and the degradable polymer material powder is 1:1-1:20.
优选的是,其中,所述生物陶瓷粉末粒径为1~300μm,生物可降解高分子材料粉末粒径为1~300μm。Preferably, the particle size of the bioceramic powder is 1-300 μm, and the particle size of the biodegradable polymer material powder is 1-300 μm.
优选的是,其中,所述生物陶瓷粉末与生物可降解高分子材料粉末的质量比为1∶1~1∶30;所述生物陶瓷粉末为生物陶瓷HA粉末或生物陶瓷BaTiO3粉末中的一种,所述可降解高分子材料粉末为可降解高分子PLA粉末或可降解高分子PGA粉末中的一种。Preferably, the mass ratio of the bioceramic powder to the biodegradable polymer powder is 1:1 to 1:30; the bioceramic powder is one of bioceramic HA powder or bioceramic BaTiO 3 powder The degradable polymer material powder is one of degradable polymer PLA powder or degradable polymer PGA powder.
优选的是,其中,进行机械球磨工艺时,设置球磨机的变频参数,先顺时针转动,转速为100~300rad/min,球磨时间为10~30min,停1~5min;再逆时针转动,转速为100~300rad/min,球磨时间为10~30min,停1~5min;循环往复,球磨总时长为3~7h,得到均匀分散的生物陶瓷-可降解高分子混合粉末。Preferably, when the mechanical ball milling process is performed, the frequency conversion parameters of the ball mill are set, firstly rotate clockwise, the rotational speed is 100-300 rad/min, the ball milling time is 10-30 minutes, and the stop is 1-5 minutes; then rotate counterclockwise, and the rotational speed is 100~300rad/min, ball milling time is 10~30min, stop for 1~5min; cycle back and forth, total ball milling time is 3~7h, obtain uniformly dispersed bioceramic-degradable polymer mixed powder.
优选的是,其中,所述真空系统的真空度为99.99%,真空干燥的温度为60~70℃,干燥时间为3~7h。Preferably, the vacuum degree of the vacuum system is 99.99%, the temperature of vacuum drying is 60-70° C., and the drying time is 3-7 hours.
优选的是,其中,所述挤出机为双螺杆挤出机,所述双螺杆挤出机的机筒包括六个温度区,从进料口向挤出口依次为第一区、第二区、第三区、第四区、第五区和第六区,其中第一区温度为100~400℃,第二区温度为100~400℃,第三区温度为100~400℃,第四区温度为100~400℃,第五区温度为100~400℃,第六区温度为100~400℃;设置预热时间为1~3h,预热温度为100~400℃。Preferably, the extruder is a twin-screw extruder, and the barrel of the twin-screw extruder includes six temperature zones, which are the first zone and the second zone from the feeding port to the extrusion port. , the third zone, the fourth zone, the fifth zone and the sixth zone, wherein the temperature of the first zone is 100~400℃, the temperature of the second zone is 100~400℃, the temperature of the third zone is 100~400℃, and the temperature of the fourth zone is 100~400℃. The temperature of the zone is 100~400℃, the temperature of the fifth zone is 100~400℃, and the temperature of the sixth zone is 100~400℃; the preheating time is set to 1~3h, and the preheat temperature is 100~400℃.
优选的是,其中,设置熔融共混的螺杆转速为10~300rad/min;物料停留时间为1~5min,熔体压力为3~15MPa;喂料速度为1~100kg/h;冷却成型系统温度为0-10℃;切粒速度为1-3m/min。Preferably, the screw speed of melt blending is set to be 10-300rad/min; the material residence time is 1-5min, the melt pressure is 3-15MPa; the feeding speed is 1-100kg/h; The temperature is 0-10℃; the cutting speed is 1-3m/min.
优选的是,其中,将生物陶瓷粉末与可降解高分子材料粉末按比例混合后,在放入球磨机前,使用分散剂对生物陶瓷粉末和可降解高分子材料粉末的混合粉末进行分散,所述分散剂的制备方法包括以下步骤:Preferably, after the bioceramic powder and the degradable polymer material powder are mixed in proportion, the mixed powder of the bioceramic powder and the degradable polymer material powder is dispersed with a dispersant before being put into the ball mill, and the The preparation method of dispersant comprises the following steps:
S1、按重量份,称取8~12份石蜡,2~4份石墨粉末,0.5~1份医用聚碳酸酯,1~1.5份聚丙烯酰胺,50~80份乙醇,4~7份氨基酸,将石蜡、医用聚碳酸酯加入至乙醇溶液中,搅拌混合均匀,得到混合溶液A,静置1~2h;S1, by weight, weigh 8-12 parts of paraffin, 2-4 parts of graphite powder, 0.5-1 part of medical polycarbonate, 1-1.5 parts of polyacrylamide, 50-80 parts of ethanol, 4-7 parts of amino acid, Add paraffin and medical polycarbonate to the ethanol solution, stir and mix evenly to obtain mixed solution A, and let stand for 1-2 hours;
S2、向混合溶液A中加入聚丙烯胺,并将溶液A升温至60~80℃,升温后以200rpm的转速进行搅拌,得到混合溶液B;混合溶液B冷却至25℃后,向其中加入石墨粉末,超声分散60~140min,超声频率为20~50kHz,得到混合浆液A;S2, add polyacrylamine to mixed solution A, and heat up solution A to 60~80 ℃, after heating up, stir at a rotating speed of 200 rpm to obtain mixed solution B; after mixed solution B is cooled to 25 ℃, add graphite to it Powder, ultrasonically disperse for 60-140min, and the ultrasonic frequency is 20-50kHz to obtain mixed slurry A;
S3、将混合浆液A加热至35~50℃,将氨基酸加入至混合浆液中,对混合浆液进行氨化,以160~300rpm的转速进行搅拌,搅拌时间20min,搅拌后静置4h,得到氨化的混合浆液B,固液分离,对固体进行烘干、粉碎,粉碎粒径为500~1000目,得到分散剂;S3. Heat the mixed slurry A to 35-50°C, add amino acids to the mixed slurry, conduct ammoniation on the mixed slurry, stir at a speed of 160-300 rpm, stir for 20 minutes, and let stand for 4 hours after stirring to obtain ammoniation The mixed slurry B is separated from solid and liquid, and the solid is dried and pulverized, and the pulverized particle size is 500-1000 mesh to obtain a dispersant;
使用分散剂对生物陶瓷粉末和可降解高分子材料粉末的混合粉末进行分散的具体方法包括;以乙醇溶液为分散介质,将混合粉末加入至乙醇溶液中,乙醇溶液的质量分数为10~30%,乙醇溶液与混合粉末的质量比为7~10∶1,向乙醇溶液中加入分散剂,并进行超声分散,超声分散频率为60~100kHz;分散时间为1~2h,得到分散的浆液;对分散浆液进行固液分离,对固体物进行烘干、粉碎,得到分散的混合粉末;The specific method of using a dispersant to disperse the mixed powder of the bioceramic powder and the degradable polymer material powder includes: using an ethanol solution as a dispersion medium, adding the mixed powder to the ethanol solution, and the mass fraction of the ethanol solution is 10-30% , the mass ratio of the ethanol solution to the mixed powder is 7-10:1, add a dispersant to the ethanol solution, and carry out ultrasonic dispersion, the ultrasonic dispersion frequency is 60-100kHz; the dispersion time is 1-2h, and the dispersed slurry is obtained; The dispersion slurry is subjected to solid-liquid separation, and the solids are dried and pulverized to obtain dispersed mixed powder;
其中,分散剂与混合粉末的质量比为1∶500~1200;所述氨基酸为色氨酸、蛋氨酸、苏氨酸、缬氨酸、赖氨酸、组氨酸、亮氨酸、异亮氨酸、丙氨酸、苯丙氨酸、胱氨酸、半胱氨酸、精氨酸中的一种。Wherein, the mass ratio of dispersant to mixed powder is 1:500-1200; the amino acids are tryptophan, methionine, threonine, valine, lysine, histidine, leucine, isoleucine One of acid, alanine, phenylalanine, cystine, cysteine, and arginine.
本发明至少包括以下有益效果:The present invention includes at least the following beneficial effects:
(1)、本发明针对单一的生物陶瓷或生物可降解高分子材料难以满足组织修复与再生的性能要求。通过将两种或多种材料复合在一起,实现材料间的优势互补,使材料的性能更优。(1) The present invention is difficult to meet the performance requirements of tissue repair and regeneration for a single bioceramic or biodegradable polymer material. By compounding two or more materials together, the advantages of the materials are complemented and the performance of the materials is better.
(2)、本发明结合机械球磨与挤出造粒工艺的优势,一方面利用机械球磨工艺强大的冲击力、剪切力和碾压力,实现陶瓷和高分子均匀混合;另一方面利用挤出造粒工艺优异的熔融、挤出、混合能力,实现陶瓷和高分子的塑化、包裹、造粒,从而制备出一种满足再生组织器官要求的复合材料。(2), the present invention combines the advantages of mechanical ball milling and extrusion granulation technology. On the one hand, the powerful impact force, shear force and rolling force of the mechanical ball milling process are used to achieve uniform mixing of ceramics and polymers; The excellent melting, extrusion and mixing capabilities of the granulation process can be achieved, and the plasticization, packaging and granulation of ceramics and polymers can be realized, thereby preparing a composite material that meets the requirements of regeneration of tissues and organs.
(3)、本发明使用分散剂对生物陶瓷粉末和可降解高分子材料粉末进行分散,提高了二者的混合均匀性,使得制备得到的复合材料具有更加优异的力学性能;其中,分散剂以石蜡和石墨粉末为主要原料,对人体无害的医用碳酸酯和聚丙酰胺为添加剂,并用氨基酸对混合浆液进行氨化,使得石蜡、医用聚碳酸酯和聚丙烯酰胺中能以少量附着或吸附形式被石墨粉末吸附,使石墨粉末颗粒度更为饱满,具有光滑的表面结构,在对复合粉末进行分散过程中,降低了生物陶瓷粉末和可降解高分子材料粉末的团聚性,因而对生物陶瓷粉末和高分子材料粉末具有很好的分散效果。(3) The present invention uses a dispersant to disperse the bioceramic powder and the degradable polymer material powder, which improves the mixing uniformity of the two, so that the prepared composite material has more excellent mechanical properties; Paraffin and graphite powder are the main raw materials, and the harmless medical carbonate and polyacrylamide are additives, and the mixed slurry is ammoniated with amino acid, so that a small amount of paraffin, medical polycarbonate and polyacrylamide can adhere or adsorb in the form of a small amount. Absorbed by graphite powder, the particle size of the graphite powder is fuller and the surface structure is smooth. During the dispersion process of the composite powder, the agglomeration of the bioceramic powder and the degradable polymer powder is reduced. And polymer material powder has a good dispersion effect.
(4)、本发明为获取最佳球磨效果,将大、中、小磨球的质量比设置为1∶1∶1~1∶5∶7,大、中、小氧化锆球直径范围分别取3~4cm,1~3cm和0~1cm,发明人发现磨球直径比例对于最终材料性能影响较大,如果大球比例过多,则研磨分散复合粉末不均匀,进而影响挤出机造粒;如果粉末大球比例过少,则球磨罐运动过程可能出现晃动,也可能出现未被球磨的大颗粒粉末。本发明使用的生物陶瓷粉末粒径为1~300μm,生物可降解高分子材料粉末粒径为1~300μm,发明人发现,生物可降解高分子材料粉末的粒径对于最终材料性能影响较大,如果粒径过大,则在形成的复合材料上掺杂不均匀,进而影响挤出机效果,最终减小复合基体的力学性能。(4), in order to obtain the best ball milling effect in the present invention, the mass ratio of large, medium and small grinding balls is set to 1:1:1~1:5:7, and the diameter ranges of large, medium and small zirconia balls are respectively taken as 3 to 4 cm, 1 to 3 cm and 0 to 1 cm, the inventors found that the ratio of the diameter of the grinding balls has a great influence on the performance of the final material. If the proportion of large balls is too large, the grinding and dispersing composite powder will be uneven, which in turn affects the granulation of the extruder; If the proportion of large powder balls is too small, there may be shaking during the movement of the ball mill, or there may be large particles of powder that have not been ball-milled. The particle size of the bioceramic powder used in the present invention is 1-300 μm, and the particle size of the biodegradable polymer material powder is 1-300 μm. The inventors found that the particle size of the biodegradable polymer material powder has a great influence on the final material properties. If the particle size is too large, the doping will be uneven on the formed composite material, thereby affecting the effect of the extruder, and finally reducing the mechanical properties of the composite matrix.
本发明使用的生物陶瓷粉末与生物可降解高分子材料粉末的质量比设置为1∶1~1∶30,发明人发现,质量比会影响复合造粒产物进行人体模拟液浸泡实验的酸碱度与降解时间。The mass ratio of the bioceramic powder and the biodegradable polymer material powder used in the present invention is set to be 1:1 to 1:30. The inventor found that the mass ratio will affect the pH and degradation of the composite granulated product in the human body simulated solution soaking experiment. time.
本发明设置球磨机的变频参数,先顺时针转动,转速为100~300rad/min,球磨时间为10-30min,停1-5min;再逆时针转动,转速为100~300rad/min,球磨时间为10-30min,停1-5min;循环往复,球磨总时长为3~7h,得到均匀分散的生物陶瓷-可降解高分子混合粉末。发明人发现,球磨设置的各个时间会影响均匀分散的效果,时间过短,会发生明显的单一材料团聚。The invention sets the frequency conversion parameters of the ball mill, firstly rotates clockwise, the rotation speed is 100-300rad/min, the ball milling time is 10-30min, and the stop is 1-5min; -30min, stop for 1-5min; cycle back and forth, the total time of ball milling is 3-7h, and a uniformly dispersed bioceramic-degradable polymer mixed powder is obtained. The inventors found that each time set by the ball milling will affect the effect of uniform dispersion, and if the time is too short, obvious single material agglomeration will occur.
本发明使用的双螺杆挤出机的机筒分为第一-第六区,第一区温度为100-400℃,第二区温度为100-400℃,第三区温度为100-400℃,第四区温度为100-400℃,第五区温度为100-400℃,第六区温度为100-4000℃;设置预热时间1-3h,预热温度为100-400℃。发明人发现,温度会影响物料是否全部熔融,进而影响是否能顺利挤出。The barrel of the twin-screw extruder used in the present invention is divided into first-sixth zones, the temperature of the first zone is 100-400°C, the temperature of the second zone is 100-400°C, and the temperature of the third zone is 100-400°C , the temperature of the fourth zone is 100-400°C, the temperature of the fifth zone is 100-400°C, and the temperature of the sixth zone is 100-4000°C; the preheating time is set to 1-3h, and the preheating temperature is 100-400°C. The inventor found that the temperature will affect whether the material is completely melted, which in turn affects whether it can be smoothly extruded.
本发明进行挤出造粒时,喂料速度设置为1-100kg/h。发明人发现,喂料速度过快,会发生螺杆堵塞。When the present invention performs extrusion granulation, the feeding speed is set to 1-100kg/h. The inventors found that if the feeding speed is too fast, the screw blockage will occur.
本发明的其它优点、目标和特征将部分通过下面的说明体现,部分还将通过对本发明的研究和实践而为本领域的技术人员所理解。Other advantages, objects, and features of the present invention will appear in part from the description that follows, and in part will be appreciated by those skilled in the art from the study and practice of the invention.
附图说明Description of drawings
图1为本发明的总结构图;Fig. 1 is the general structure diagram of the present invention;
图2为本发明的双进出冷却管结构图;Fig. 2 is the structure diagram of double inlet and outlet cooling pipes of the present invention;
图3为本发明的进料单元详细结构图;Fig. 3 is the detailed structure diagram of the feeding unit of the present invention;
图4为本发明的匀料台俯视结构图;Fig. 4 is the top plan view of the screed table of the present invention;
图5为本发明的配料箱俯视结构图;Fig. 5 is the top view structure diagram of the batching box of the present invention;
图6为本发明的推拉板俯视结构图;FIG. 6 is a top plan view of the push-pull plate of the present invention;
图7为本发明的双螺杆其中一个的侧面结构图;Fig. 7 is a side structural view of one of the twin screws of the present invention;
图8为本发明的双螺杆其中一个的外花键键齿。Fig. 8 shows the external spline teeth of one of the twin screws of the present invention.
具体实施方式Detailed ways
下面对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。The present invention will be further described in detail below, so that those skilled in the art can implement it with reference to the description.
应当理解,本文所使用的诸如“具有”、“包含”以及“包括”术语并不排除一个或多个其它元件或其组合的存在或添加。It should be understood that terms such as "having", "comprising" and "including" as used herein do not exclude the presence or addition of one or more other elements or combinations thereof.
需要说明的是,在本发明的描述中,术语指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本发明和简化描述,并不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性。It should be noted that, in the description of the present invention, the azimuth or positional relationship indicated by the terms is based on the azimuth or positional relationship shown in the accompanying drawings, which is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that A device or element must have a particular orientation, be constructed and operate in a particular orientation, and therefore should not be construed as limiting the invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed to indicate or imply relative importance.
在本发明的描述中,除非另有明确的规定和限定,术语“安装”、“设置有”、“套设/接”、“连接”等,应做广义理解,例如“连接”,可以是固定连接,也可以是可拆卸连接,或一体地连接,可以是机械连接,也可以是电连接,可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通,对于本领域的普通技术人员而言,可以具体情况理解上述术语在本发明中的具体含义。In the description of the present invention, unless otherwise expressly specified and limited, the terms "installed", "provided with", "sleeved/connected", "connected", etc., should be understood in a broad sense, for example, "connected" may be A fixed connection can also be a detachable connection, or an integral connection, a mechanical connection, an electrical connection, a direct connection, an indirect connection through an intermediate medium, or an internal connection between two components. Those of ordinary skill in the art can understand the specific meanings of the above terms in the present invention in specific situations.
此外,在本发明中,除非另有明确的规定和限定,第一特征在第二特征“上”或“下”可以是第一和第二特征直接接触,或第一和第二特征通过中间媒介间接接触。而且,第一特征在第二特征“之上”、“上方”和“上面”可是第一特征在第二特征正上方或斜上方,或仅仅表示第一特征水平高度高于第二特征。第一特征在第二特征“之下”、“下方”和“下面”可以是第一特征在第二特征正下方或斜下方,或仅仅表示第一特征水平高度小于第二特征。In addition, in the present invention, unless otherwise expressly specified and limited, a first feature "on" or "under" a second feature may be in direct contact with the first and second features, or the first and second features through the middle indirect contact with the media. Also, the first feature being "above", "over" and "above" the second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is level higher than the second feature. The first feature being "below", "below" and "below" the second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature has a lower level than the second feature.
实施例1:Example 1:
按1:9的质量比分布称取粒径10um的0.1kg生物陶瓷HA粉末与粒径20um的0.9kg生物可降解高分子材料PLA粉末,将两者加入到球磨罐中并加入大、中、小磨球质量比1:1:1(球料比为1:1)。先顺时针转速为100rad/min,球磨时间为10min,停1min;再逆时针转动,转速为100rad/min,球磨时间为10min,停1min;循环往复;球磨总时长为3h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为170℃,第二区温度为175℃,第三区温度为170℃,第四区温度为160℃,第五区温度为180℃,第六区温度为160℃;预热时间1h;预热温度为160℃;熔融共混的螺杆转速为50rad/min;物料停留时间为1min;熔体压力为3MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Weigh 0.1kg of bioceramic HA powder with a particle size of 10um and 0.9kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 1:9, add the two into the ball mill and add the large, medium and The mass ratio of small grinding balls is 1:1:1 (the ratio of balls to material is 1:1). First, the clockwise rotation speed is 100rad/min, the ball milling time is 10min, and the stop is 1min; then the counterclockwise rotation speed is 100rad/min, the ball milling time is 10min, and the stoppage time is 1min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first-sixth zone of the barrel of the twin-screw extruder, the temperature of the first zone is 170 ℃, the temperature of the second zone is 175 ℃, the temperature of the third zone is 170 ℃, The temperature of the fourth zone is 160°C, the temperature of the fifth zone is 180°C, and the temperature of the sixth zone is 160°C; the preheating time is 1h; the preheating temperature is 160°C; the screw speed of melt blending is 50rad/min; the material residence time is 1min; the melt pressure is 3MPa; the feeding speed is 10kg/h; the temperature of the cooling and forming system is 3℃; the cutting speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末可以大部分分散均匀,出现少量HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and the PLA powder could be mostly uniformly dispersed, and a small amount of HA self-agglomeration and PLA self-agglomeration appeared.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条基本光滑,直径为3mm,但会出现断断续续的出丝现象。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are basically smooth, with a diameter of 3mm, but there will be intermittent filaments.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为4.0,小于人体体液的酸碱度;降解时间为6个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 of the degradation product, and the soaking temperature was 37 °C. pH; degradation time is 6 months.
复合造粒产物进行力学性能测试,压缩强度为8MPa,拉伸强度为6MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 8 MPa and the tensile strength was 6 MPa.
实施例2:Example 2:
按1:4的质量比分布称取粒径10um的0.2kg生物陶瓷HA粉末与粒径20um的0.8kg生物可降解高分子材料PLA粉末,将两者加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为100rad/min,球磨时间为10min,停1min;再逆时针转动,转速为100rad/min,球磨时间为10min,停1min;循环往复;球磨总时长为3h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为170℃,第二区温度为175℃,第三区温度为170℃,第四区温度为160℃,第五区温度为180℃,第六区温度为160℃;预热时间1h;预热温度为160℃;熔融共混的螺杆转速为50rad/min;物料停留时间为1min;熔体压力为3MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Weigh 0.2kg of bioceramic HA powder with a particle size of 10um and 0.8kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 1:4, add the two into the ball mill and add the large, medium and The mass ratio of small grinding balls is 1:3:5 (the ratio of balls to material is 1:1). First, the clockwise rotation speed is 100rad/min, the ball milling time is 10min, and the stop is 1min; then the counterclockwise rotation speed is 100rad/min, the ball milling time is 10min, and the stoppage time is 1min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first-sixth zone of the barrel of the twin-screw extruder, the temperature of the first zone is 170 ℃, the temperature of the second zone is 175 ℃, the temperature of the third zone is 170 ℃, The temperature of the fourth zone is 160°C, the temperature of the fifth zone is 180°C, and the temperature of the sixth zone is 160°C; the preheating time is 1h; the preheating temperature is 160°C; the screw speed of melt blending is 50rad/min; the material residence time is 1min; the melt pressure is 3MPa; the feeding speed is 10kg/h; the temperature of the cooling and forming system is 3℃; the cutting speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末基本分散均匀,少量出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and the PLA powder were basically uniformly dispersed, and a small amount of HA self-agglomeration and PLA self-agglomeration occurred.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3mm,但时常会出现断断续续的出丝现象。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3mm, but intermittent filaments often appear.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为6.2,略小于人体体液的酸碱度;降解时间为7个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 for degradation products, and the soaking temperature was 37 °C. After soaking for 28 days, the test pH value was 6.2, which was slightly smaller than that of human body fluids. pH; degradation time is 7 months.
复合造粒产物进行力学性能测试,压缩强度为10.0MPa,拉伸强度为8.7MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 10.0 MPa and the tensile strength was 8.7 MPa.
实施例3:Example 3:
按1:4的质量比分布称取粒径10um的0.2kg生物陶瓷HA粉末与粒径20um的0.8kg生物可降解高分子材料PLA粉末,将两者加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为200rad/min,球磨时间为20min,停2min;再逆时针转动,转速为200rad/min,球磨时间为20min,停2min;循环往复;球磨总时长为4h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为170℃,第二区温度为175℃,第三区温度为170℃,第四区温度为160℃,第五区温度为180℃,第六区温度为160℃;预热时间1h;预热温度为160℃;熔融共混的螺杆转速为50rad/min;物料停留时间为1min;熔体压力为3MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Weigh 0.2kg of bioceramic HA powder with a particle size of 10um and 0.8kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 1:4, add the two into the ball mill and add the large, medium and The mass ratio of small grinding balls is 1:3:5 (the ratio of balls to material is 1:1). First, the clockwise speed is 200rad/min, the ball milling time is 20min, and the stop is 2min; then the counterclockwise rotation is 200rad/min, the ball milling time is 20min, and the stop is 2min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first-sixth zone of the barrel of the twin-screw extruder, the temperature of the first zone is 170 ℃, the temperature of the second zone is 175 ℃, the temperature of the third zone is 170 ℃, The temperature of the fourth zone is 160°C, the temperature of the fifth zone is 180°C, and the temperature of the sixth zone is 160°C; the preheating time is 1h; the preheating temperature is 160°C; the screw speed of melt blending is 50rad/min; the material residence time is 1min; the melt pressure is 3MPa; the feeding speed is 10kg/h; the temperature of the cooling and forming system is 3℃; the cutting speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末基本分散均匀,未出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and the PLA powder were basically uniformly dispersed, and there was no self-agglomeration of HA and PLA.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3mm,但时常会出现断断续续的出丝现象。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3mm, but intermittent filaments often appear.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为6.15,略小于人体体液的酸碱度;降解时间为7个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 for degradation products, and the soaking temperature was 37 °C. After soaking for 28 days, the test pH value was 6.15, which was slightly smaller than that of human body fluids. pH; degradation time is 7 months.
复合造粒产物进行力学性能测试,压缩强度为11.2MPa,拉伸强度为9.6MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 11.2 MPa and the tensile strength was 9.6 MPa.
实施例4:Example 4:
按1:4的质量比分布称取粒径10um的0.2kg生物陶瓷HA粉末与粒径20um的0.8kg生物可降解高分子材料PLA粉末,将两者加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为200rad/min,球磨时间为20min,停2min;再逆时针转动,转速为200rad/min,球磨时间为20min,停2min;循环往复;球磨总时长为4h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为180℃,第二区温度为185℃,第三区温度为185℃,第四区温度为185℃,第五区温度为190℃,第六区温度为190℃;预热时间1.5h;预热温度为190℃;熔融共混的螺杆转速为50rad/min;物料停留时间为1min;熔体压力为3MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Weigh 0.2kg of bioceramic HA powder with a particle size of 10um and 0.8kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 1:4, add the two into the ball mill and add the large, medium and The mass ratio of small grinding balls is 1:3:5 (the ratio of balls to material is 1:1). First, the clockwise speed is 200rad/min, the ball milling time is 20min, and the stop is 2min; then the counterclockwise rotation is 200rad/min, the ball milling time is 20min, and the stop is 2min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first to sixth zones of the barrel of the twin-screw extruder, the temperature of the first zone is 180 ° C, the temperature of the second zone is 185 ° C, the temperature of the third zone is 185 ° C, The temperature of the fourth zone is 185°C, the temperature of the fifth zone is 190°C, and the temperature of the sixth zone is 190°C; the preheating time is 1.5h; the preheating temperature is 190°C; the screw speed of melt blending is 50rad/min; the material residence time The melt pressure is 3MPa; the feeding speed is 10kg/h; the cooling and forming system temperature is 3℃; the pelletizing speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末基本分散均匀,未出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and the PLA powder were basically uniformly dispersed, and there was no self-agglomeration of HA and PLA.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3mm,但偶尔会出现断断续续的出丝现象。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3mm, but occasionally there will be intermittent filaments.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为6.15,略小于人体体液的酸碱度;降解时间为7个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 for degradation products, and the soaking temperature was 37 °C. After soaking for 28 days, the test pH value was 6.15, which was slightly smaller than that of human body fluids. pH; degradation time is 7 months.
复合造粒产物进行力学性能测试,压缩强度为11.5MPa,拉伸强度为9.7MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 11.5 MPa and the tensile strength was 9.7 MPa.
实施例5:Example 5:
按1:4的质量比分布称取粒径10um的0.2kg生物陶瓷HA粉末与粒径20um的0.8kg生物可降解高分子材料PLA粉末,将两者加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为200rad/min,球磨时间为20min,停2min;再逆时针转动,转速为200rad/min,球磨时间为20min,停2min;循环往复;球磨总时长为4h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为180℃,第二区温度为185℃,第三区温度为185℃,第四区温度为185℃,第五区温度为190℃,第六区温度为190℃;预热时间1.5h;预热温度为190℃;熔融共混的螺杆转速为50rad/min;物料停留时间为3min;熔体压力为4MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Weigh 0.2kg of bioceramic HA powder with a particle size of 10um and 0.8kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 1:4, add the two into the ball mill and add the large, medium and The mass ratio of small grinding balls is 1:3:5 (the ratio of balls to material is 1:1). First, the clockwise speed is 200rad/min, the ball milling time is 20min, and the stop is 2min; then the counterclockwise rotation is 200rad/min, the ball milling time is 20min, and the stop is 2min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first to sixth zones of the barrel of the twin-screw extruder, the temperature of the first zone is 180 ° C, the temperature of the second zone is 185 ° C, the temperature of the third zone is 185 ° C, The temperature of the fourth zone is 185°C, the temperature of the fifth zone is 190°C, and the temperature of the sixth zone is 190°C; the preheating time is 1.5h; the preheating temperature is 190°C; the screw speed of melt blending is 50rad/min; the material residence time The melt pressure is 4MPa; the feeding speed is 10kg/h; the cooling and forming system temperature is 3℃; the pelletizing speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末基本分散均匀,未出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and the PLA powder were basically uniformly dispersed, and there was no self-agglomeration of HA and PLA.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3mm,出丝流畅。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3mm, and the strands are smooth.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为6.15,略小于人体体液的酸碱度;降解时间为7个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 for degradation products, and the soaking temperature was 37 °C. After soaking for 28 days, the test pH value was 6.15, which was slightly smaller than that of human body fluids. pH; degradation time is 7 months.
复合造粒产物进行力学性能测试,压缩强度为11.7MPa,拉伸强度为9.9MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 11.7 MPa and the tensile strength was 9.9 MPa.
实施例6:Example 6:
按3:7的质量比分布称取粒径10um的0.3kg生物陶瓷HA粉末与粒径20um的0.7kg生物可降解高分子材料PLA粉末,将两者加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为200rad/min,球磨时间为20min,停2min;再逆时针转动,转速为200rad/min,球磨时间为20min,停2min;循环往复;球磨总时长为4h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为180℃,第二区温度为185℃,第三区温度为185℃,第四区温度为185℃,第五区温度为190℃,第六区温度为190℃;预热时间1.5h;预热温度为190℃;熔融共混的螺杆转速为50rad/min;物料停留时间为3min;熔体压力为4MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。According to the mass ratio of 3:7, weigh 0.3kg bioceramic HA powder with a particle size of 10um and 0.7kg biodegradable polymer material PLA powder with a particle size of 20um, add the two into the ball mill and add the large, medium, and The mass ratio of small grinding balls is 1:3:5 (the ratio of balls to material is 1:1). First, the clockwise speed is 200rad/min, the ball milling time is 20min, and the stop is 2min; then the counterclockwise rotation is 200rad/min, the ball milling time is 20min, and the stop is 2min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first to sixth zones of the barrel of the twin-screw extruder, the temperature of the first zone is 180 ° C, the temperature of the second zone is 185 ° C, the temperature of the third zone is 185 ° C, The temperature of the fourth zone is 185°C, the temperature of the fifth zone is 190°C, and the temperature of the sixth zone is 190°C; the preheating time is 1.5h; the preheating temperature is 190°C; the screw speed of melt blending is 50rad/min; the material residence time The melt pressure is 4MPa; the feeding speed is 10kg/h; the cooling and forming system temperature is 3℃; the pelletizing speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末基本分散均匀,未出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and the PLA powder were basically uniformly dispersed, and there was no self-agglomeration of HA and PLA.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3mm,出丝流畅。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3mm, and the strands are smooth.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为7.3,属于人体体液的酸碱度;降解时间为10个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 of the degradation product, the soaking temperature was 37 °C, and after soaking for 28 days, the test pH value was 7.3, which belongs to human body fluid pH; degradation time is 10 months.
复合造粒产物进行力学性能测试,压缩强度为15MPa,拉伸强度为10.9MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 15 MPa and the tensile strength was 10.9 MPa.
实施例7Example 7
按3:7的质量比分布称取粒径10um的0.3kg生物陶瓷HA粉末与粒径20um的0.7kg生物可降解高分子材料PLA粉末,使用分散剂对生物陶瓷HA粉末和生物可降解高分子材料PLA粉末的混合粉末进行分散,所述分散剂的制备方法包括以下步骤:Weigh 0.3kg of bioceramic HA powder with a particle size of 10um and 0.7kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 3:7. The mixed powder of the material PLA powder is dispersed, and the preparation method of the dispersant comprises the following steps:
S1、按重量份,称取8g石蜡,2g石墨粉末,0.5g医用聚碳酸酯,1g聚丙烯酰胺,150g乙醇,4g份丙氨酸,将石蜡、医用聚碳酸酯加入至乙醇溶液中,搅拌混合均匀,得到混合溶液A,静置1h;S1. Weigh 8g of paraffin, 2g of graphite powder, 0.5g of medical polycarbonate, 1g of polyacrylamide, 150g of ethanol, and 4g of alanine by weight, add paraffin and medical polycarbonate to the ethanol solution, and stir Mix evenly to obtain mixed solution A, which is left to stand for 1 hour;
S2、向混合溶液A中加入聚丙烯胺,并将溶液A升温至60℃,升温后以200rpm的转速进行搅拌,得到混合溶液B;混合溶液B冷却至25℃后,向其中加入石墨粉末,超声分散60min,超声频率为20kHz,得到混合浆液A;S2. Add polyacrylamine to the mixed solution A, and heat the solution A to 60° C., and stir at a rotational speed of 200 rpm after heating to obtain a mixed solution B; after the mixed solution B is cooled to 25° C., add graphite powder to it, Ultrasonic dispersion was carried out for 60 min, and the ultrasonic frequency was 20 kHz to obtain mixed slurry A;
S3、将混合浆液A加热至35℃,将丙氨酸加入至混合浆液中,对混合浆液进行氨化,以160rpm的转速进行搅拌,搅拌时间20min,搅拌后静置4h,得到氨化的混合浆液B,固液分离,对固体进行烘干、粉碎,粉碎粒径为500目,得到分散剂;S3. Heat the mixed slurry A to 35°C, add alanine to the mixed slurry, aminate the mixed slurry, stir at a speed of 160 rpm, stir for 20 min, and let stand for 4 h after stirring to obtain an ammoniated mixture Slurry B, solid-liquid separation, drying and pulverizing the solid, and the pulverized particle size is 500 meshes to obtain a dispersant;
使用分散剂对生物陶瓷粉末和可降解高分子材料粉末的混合粉末进行分散的具体方法包括;以乙醇溶液为分散介质,将混合粉末加入至乙醇溶液中,乙醇溶液的质量分数为20%,乙醇溶液用量为7kg,向乙醇溶液中加入2g分散剂,并进行超声分散,超声分散频率为60kHz;分散时间为1h,得到分散的浆液;对分散浆液进行固液分离,对固体物进行烘干、粉碎,得到分散的混合粉末;The specific method of using a dispersant to disperse the mixed powder of the bioceramic powder and the degradable polymer material powder includes: using an ethanol solution as a dispersion medium, adding the mixed powder to the ethanol solution, the mass fraction of the ethanol solution is 20%, and the ethanol solution is 20%. The dosage of the solution is 7kg, 2g of dispersant is added to the ethanol solution, and ultrasonic dispersion is carried out, and the ultrasonic dispersion frequency is 60kHz; the dispersion time is 1h, and a dispersed slurry is obtained; Pulverized to obtain dispersed mixed powder;
将分散的混合粉末加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为200rad/min,球磨时间为20min,停2min;再逆时针转动,转速为200rad/min,球磨时间为20min,停2min;循环往复;球磨总时长为4h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机第一区-第六区的温度,第一区温度为180℃,第二区温度为185℃,第三区温度为185℃,第四区温度为185℃,第五区温度为190℃,第六区温度为190℃;预热时间1.5h;预热温度为190℃;熔融共混的螺杆转速为50rad/min;物料停留时间为3min;熔体压力为4MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Add the dispersed mixed powder into the ball mill tank and add the large, medium and small grinding balls in a mass ratio of 1:3:5 (the ball-to-material ratio is 1:1). First, the clockwise speed is 200rad/min, the ball milling time is 20min, and the stop is 2min; then the counterclockwise rotation is 200rad/min, the ball milling time is 20min, and the stop is 2min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first zone to the sixth zone of the twin-screw extruder, the temperature of the first zone is 180 ° C, the temperature of the second zone is 185 ° C, the temperature of the third zone is 185 ° C, and the temperature of the first zone is 185 ° C. The temperature of the fourth zone is 185°C, the temperature of the fifth zone is 190°C, and the temperature of the sixth zone is 190°C; the preheating time is 1.5h; the preheating temperature is 190°C; the screw speed of melt blending is 50rad/min; the material residence time The melt pressure is 4MPa; the feeding speed is 10kg/h; the cooling and forming system temperature is 3℃; the pelletizing speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末具有很好的分散均匀性,未出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and PLA powder had good dispersion uniformity, and there was no self-agglomeration of HA and PLA.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3m,出丝流畅。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3m and smooth strands.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为7.3,属于人体体液的酸碱度;降解时间为7个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 of the degradation product, the soaking temperature was 37 °C, and after soaking for 28 days, the test pH value was 7.3, which belongs to human body fluid pH; degradation time is 7 months.
复合造粒产物进行力学性能测试,压缩强度为22MPa,拉伸强度为11.8MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 22 MPa and the tensile strength was 11.8 MPa.
实施例8Example 8
按3:7的质量比分布称取粒径10um的0.3kg生物陶瓷HA粉末与粒径20um的0.7kg生物可降解高分子材料PLA粉末,使用分散剂对生物陶瓷HA粉末和生物可降解高分子材料PLA粉末的混合粉末进行分散,所述分散剂的制备方法包括以下步骤:Weigh 0.3kg of bioceramic HA powder with a particle size of 10um and 0.7kg of biodegradable polymer material PLA powder with a particle size of 20um according to the mass ratio of 3:7. The mixed powder of the material PLA powder is dispersed, and the preparation method of the dispersant comprises the following steps:
S1、按重量份,称取12g石蜡,4g石墨粉末,1g医用聚碳酸酯,1.5g聚丙烯酰胺,80g乙醇,7g赖氨酸,将石蜡、医用聚碳酸酯加入至乙醇溶液中,搅拌混合均匀,得到混合溶液A,静置2h;S1. Weigh 12g of paraffin, 4g of graphite powder, 1g of medical polycarbonate, 1.5g of polyacrylamide, 80g of ethanol, 7g of lysine by weight, add paraffin and medical polycarbonate to the ethanol solution, stir and mix Evenly, get mixed solution A, let stand for 2h;
S2、向混合溶液A中加入聚丙烯胺,并将溶液A升温至80℃,升温后以200rpm的转速进行搅拌,得到混合溶液B;混合溶液B冷却至25℃后,向其中加入石墨粉末,超声分散140min,超声频率为50kHz,得到混合浆液A;S2. Add polyacrylamine to the mixed solution A, and heat the solution A to 80° C. After heating up, stir at a rotational speed of 200 rpm to obtain a mixed solution B; after the mixed solution B is cooled to 25° C., add graphite powder to it, Ultrasonic dispersion was carried out for 140 min, and the ultrasonic frequency was 50 kHz to obtain mixed slurry A;
S3、将混合浆液A加热至50℃,将赖氨酸加入至混合浆液中,对混合浆液进行氨化,以300rpm的转速进行搅拌,搅拌时间20min,搅拌后静置4h,得到氨化的混合浆液B,固液分离,对固体进行烘干、粉碎,粉碎粒径为1000目,得到分散剂;S3. Heat the mixed slurry A to 50°C, add lysine to the mixed slurry, aminate the mixed slurry, stir at a speed of 300 rpm, stir for 20 minutes, and let stand for 4 hours after stirring to obtain an ammoniated mixture Slurry B, solid-liquid separation, drying and pulverizing the solid, and the pulverized particle size is 1000 mesh to obtain a dispersant;
使用分散剂对生物陶瓷粉末和可降解高分子材料粉末的混合粉末进行分散的具体方法包括;以乙醇溶液为分散介质,将混合粉末加入至乙醇溶液中,乙醇溶液的质量分数为30%,乙醇溶液用量为10kg,向乙醇溶液中加入1g分散剂,并进行超声分散,超声分散频率为100kHz;分散时间为2h,得到分散的浆液;对分散浆液进行固液分离,对固体物进行烘干、粉碎,得到分散的混合粉末;The specific method of using a dispersant to disperse the mixed powder of the bioceramic powder and the degradable polymer material powder includes: using an ethanol solution as a dispersion medium, adding the mixed powder to the ethanol solution, the mass fraction of the ethanol solution is 30%, and the ethanol solution is 30%. The dosage of the solution is 10kg, 1g of dispersant is added to the ethanol solution, and ultrasonic dispersion is performed, and the frequency of ultrasonic dispersion is 100kHz; the dispersion time is 2h, and a dispersed slurry is obtained; Pulverized to obtain dispersed mixed powder;
将分散的混合粉末加入到球磨罐中并加入大、中、小磨球质量比1:3:5(球料比为1:1)。先顺时针转速为200rad/min,球磨时间为20min,停2min;再逆时针转动,转速为200rad/min,球磨时间为20min,停2min;循环往复;球磨总时长为4h,得到生物陶瓷-可降解高分子混合粉末。以上述复合粉末为原料,设置双螺杆挤出机的机筒第一-第六区的温度,第一区温度为180℃,第二区温度为185℃,第三区温度为185℃,第四区温度为185℃,第五区温度为190℃,第六区温度为190℃;预热时间1.5h;预热温度为190℃;熔融共混的螺杆转速为50rad/min;物料停留时间为3min;熔体压力为4MPa;喂料速度为10kg/h;冷却成型系统温度为3℃;切粒速度为1m/min。Add the dispersed mixed powder into the ball mill tank and add the large, medium and small grinding balls in a mass ratio of 1:3:5 (the ball-to-material ratio is 1:1). First, the clockwise speed is 200rad/min, the ball milling time is 20min, and the stop is 2min; then the counterclockwise rotation is 200rad/min, the ball milling time is 20min, and the stop is 2min; Degradable polymer mixed powder. Using the above-mentioned composite powder as the raw material, set the temperature of the first to sixth zones of the barrel of the twin-screw extruder, the temperature of the first zone is 180 ° C, the temperature of the second zone is 185 ° C, the temperature of the third zone is 185 ° C, The temperature of the fourth zone is 185°C, the temperature of the fifth zone is 190°C, and the temperature of the sixth zone is 190°C; the preheating time is 1.5h; the preheating temperature is 190°C; the screw speed of melt blending is 50rad/min; the material residence time The melt pressure is 4MPa; the feeding speed is 10kg/h; the cooling and forming system temperature is 3℃; the pelletizing speed is 1m/min.
在进行微观结构测试发现,HA粉末与PLA粉末具有很好的分散均匀性,未出现HA自行团聚与PLA自行团聚。In the microstructure test, it was found that the HA powder and PLA powder had good dispersion uniformity, and there was no self-agglomeration of HA and PLA.
球磨后的复合粉末在双螺杆挤出机上可以挤出,挤出丝条光滑,直径为3mm,出丝流畅。The ball-milled composite powder can be extruded on a twin-screw extruder, and the extruded strands are smooth, with a diameter of 3mm, and the strands are smooth.
对制备的复合造粒产物进行人体模拟液浸泡实验,被浸泡材料与人体模拟液体积比为降解产物1:5,浸泡温度为37℃,浸泡28天后,测试PH值为7.3,属于人体体液的酸碱度;降解时间为8个月。The prepared composite granulation product was subjected to a human body simulated solution soaking experiment. The volume ratio of the material to be soaked to the human body simulated solution was 1:5 of the degradation product, the soaking temperature was 37 °C, and after soaking for 28 days, the test pH value was 7.3, which belongs to human body fluid pH; degradation time is 8 months.
复合造粒产物进行力学性能测试,压缩强度为23MPa,拉伸强度为12.1MPa。The mechanical properties of the composite granulated product were tested, and the compressive strength was 23 MPa and the tensile strength was 12.1 MPa.
图1-8示出了实施例1-实施例8所使用的双螺杆挤出机的结构示意图,包括:Figures 1-8 show the schematic structural diagrams of the twin-screw extruders used in Examples 1-8, including:
分段式机筒1,其包括多个间隔配置的加热机筒11;多个所述加热机筒11之间设置有冷却单元2;所述分段式机筒1输入端设置有用于导入物料的进料单元3;所述分段式机筒1内部设置有用于导出物料的挤出单元4。The segmented barrel 1 includes a plurality of heating barrels 11 arranged at intervals; a cooling unit 2 is arranged between the plurality of the heating barrels 11; The feeding unit 3; the segmented barrel 1 is provided with an extrusion unit 4 for exporting materials.
工作原理:在使用本发明时,将待加工物料导入进料单元3,进料单元3件将物料陆续送入分段式筒体1中,安装预先设定好的各级加热机筒11的加热温度,加热机筒11内部的加热装置对物料进行均匀的加热融化,并通过挤出单元4对物料一边均匀搅拌,一边挤出,间隔设置的冷却单元2开始启动制冷,对各级加热机筒11的进行相应的冷却降温,让物料在整个熔融搅拌挤出的流程中,按照加热→降温→加热→降温等流程在分段式机筒1循环作业,最后直至完成熔融的物料导出,最后将物料送出即可。图1所示的双螺杆挤出机设置有6个加热机筒11,从右向左依次对应对生物陶瓷-可降解高分子混合粉末进行加热熔融的第一温度区、第二温度区、第三温度区、第四温度区、第五温度区和第六温度区。Working principle: When using the present invention, the materials to be processed are introduced into the feeding unit 3, and the 3 feeding units successively feed the materials into the segmented cylinder 1, and install the pre-set heating cylinders 11 at all levels. Heating temperature, the heating device inside the heating barrel 11 uniformly heats and melts the material, and extrudes the material while evenly stirring the material through the extrusion unit 4. The barrel 11 is cooled and cooled accordingly, so that the material is circulated in the segmented barrel 1 according to the process of heating→cooling→heating→cooling in the whole process of melting, stirring and extrusion, and finally until the molten material is exported, and finally Just send the material. The twin-screw extruder shown in FIG. 1 is provided with 6 heating barrels 11, which correspond to the first temperature zone, the second temperature zone, the Three temperature zones, fourth temperature zone, fifth temperature zone and sixth temperature zone.
这种技术方案的优点在于:本发明采用分段式机筒1中的多个加热机筒11配合间隔设置的冷却单元2,实现了不同加工区段(加热机筒11)温度的精确独立控制,解决了传统熔融物料挤出工艺中因无法快速温度响应而造成局部高温降解的共性问题,从而能够以高稳定性和高生产率制造具有均匀物性的生物陶瓷-可降解高分子混合粉末。The advantage of this technical solution is that the present invention adopts the plurality of heating barrels 11 in the segmented barrel 1 to cooperate with the cooling units 2 arranged at intervals, so as to realize precise and independent temperature control of different processing sections (heating barrels 11 ). , which solves the common problem of local high temperature degradation caused by the inability of rapid temperature response in the traditional molten material extrusion process, so that the bioceramic-degradable polymer mixed powder with uniform physical properties can be produced with high stability and high productivity.
在上述技术方案中,所述冷却单元2包括:多个所述加热机筒11之间设置有冷却机筒21;多个所述冷却机筒21下端共同连接有可循环式收排液的冷却水箱22;所述冷却水箱22内部设置有水泵,且输入端与输出端分别连接有冷却进水总管23与冷却出水总管24;所述冷却进水总管23与冷却出水总管24之间设置有内置多条水路的冷却歧管25;多个所述冷却机筒21与冷却歧管25之间分别设置有双进出冷却管26;所述双进出冷却管26分别包括一个内冷却管261和外冷却管262;所述内冷却管261两端(即进水端、出水端)对接至冷却歧管25;所述内冷却管261中部绕卷成多圈,且贴合固定在冷却机筒21外壁;所述外冷却管262两端(即进水端、出水端)对接至冷却歧管25;所述外冷却管262中部绕卷成多圈,且贴合固定在内冷却管261外层,形成了双进双出的冷却水道;所述内冷却管261与外冷却管262的两端沿冷却机筒21轴线前后排列设置,且均位冷却机筒21的同侧。In the above technical solution, the cooling unit 2 includes: a cooling barrel 21 is arranged between a plurality of the heating barrels 11; Water tank 22; a water pump is provided inside the cooling water tank 22, and a cooling water inlet main pipe 23 and a cooling water outlet main pipe 24 are respectively connected to the input end and the output end; a built-in cooling water inlet pipe 23 and the cooling water outlet main pipe 24 are arranged between the cooling water main pipe 23 and the cooling water outlet main pipe 24 cooling manifolds 25 of multiple water circuits; dual inlet and outlet cooling pipes 26 are respectively provided between the plurality of cooling barrels 21 and the cooling manifolds 25; the dual inlet and outlet cooling pipes 26 respectively include an inner cooling pipe 261 and an outer cooling pipe Pipe 262; both ends of the inner cooling pipe 261 (ie, the water inlet end and the water outlet end) are butted to the cooling manifold 25; the middle of the inner cooling pipe 261 is wound into multiple circles, and is fitted and fixed to the outer wall of the cooling barrel 21 ; The two ends of the outer cooling pipe 262 (ie the water inlet end and the water outlet end) are butted to the cooling manifold 25; A double-in and double-out cooling water channel is formed; both ends of the inner cooling pipe 261 and the outer cooling pipe 262 are arranged in front and back along the axis of the cooling barrel 21 , and the cooling barrel 21 is on the same side.
这种技术方案的优势在于:The advantages of this technical solution are:
(1)冷却单元2中的各个部件共同组成了“双进双出”水道系统,进一步提高了每个冷却机筒21的冷却效率,配合分段式机筒1,解决了传统工艺下,生物陶瓷-可降解高分子混合粉末的熔融挤出因无法快速温度响应而造成局部高温降解的共性问题,让处于分段式机筒1中的物料,能够在间隔设置的冷却机筒21的进行不同程度的冷却,通过这样一种工艺,能够显著提高生物陶瓷-可降解高分子混合粉末熔融挤出的制备效率和成品品质;(1) The various components in the cooling unit 2 together form a "double-in and double-out" water channel system, which further improves the cooling efficiency of each cooling
(2)这种双进双出水道,相比于单水道冷却,传递热量效果更好;同时,采用这种外圈包裹内圈的双进出冷却管26,其意义在于,外圈的出水端能够带走内圈的热量,冷却进水端能够带走冷却出水端的热量,为一种循环冷却模式,这样传递热量效果更好,筒体冷却均匀,不易发生变形;(2) Compared with the single-channel cooling, this kind of double-inlet and double-outlet cooling pipes has better heat transfer effect; at the same time, the use of the double-inlet-outlet cooling pipe 26 with the outer ring wrapping the inner ring means that the water outlet end of the outer ring is used for cooling. It can take away the heat of the inner ring, and the cooling water inlet end can take away the heat of the cooling water outlet end, which is a circulating cooling mode, so that the heat transfer effect is better, the cylinder body is cooled evenly, and it is not easy to deform;
(3)同时双进出冷却管26所具有的双水道,是关于冷却机筒21轴线前后排列的,相比较传统双水道的左右排列,冷却区域的长度没有增加,但节省了安装空间,也节省了材料成本。(3) At the same time, the dual water channels of the dual inlet and outlet cooling pipes 26 are arranged in the front and rear of the axis of the cooling
在上述技术方案中,所述进料单元3包括一个配料桶31;所述配料桶31内置四个上端开口的导料仓32;四个所述导料仓32中部一体连接有支撑柱321;四个所述导料仓32底部向中倾斜,统一汇聚形成漏口,并向下延伸形成排料管322;所述漏口间隔设置于支撑柱321下方;四个所述导料仓32底部上方可滑动设置有可向外部抽出的分阶出料板33;四个所述导料仓32底部上方两侧设置有滑槽Ⅰ;四个所述分阶出料板33两侧设置有可分别嵌入两个滑槽Ⅰ的滑条Ⅰ,从而形成了滑动连接;所述支撑柱321下端设置有多个限位槽320;四个所述分阶出料板33前端设置有把手;四个所述分阶出料板后端设置有卡入限位槽320的楔块330;四个所述分阶出料板33间隔设置有四个定位销孔331;四个所述导料仓32侧面设置有竖向向下,且与四个定位销孔331相匹配的的滑动插销323。In the above technical solution, the feeding unit 3 includes a batching bucket 31; the batching bucket 31 has four built-in guide bins 32 with upper ends open; the middle of the four guide bins 32 is integrally connected with a support column 321; The bottoms of the four guide bins 32 are slanted toward the middle, converge together to form leaks, and extend downward to form discharge pipes 322; the leaks are arranged at intervals below the support column 321; the bottoms of the four guide bins 32 The upper part is slidably provided with a step-by-step discharge plate 33 that can be pulled out to the outside; four sides of the bottom of the four guide bins 32 are provided with chute I; The slide bars I of the two chutes I are respectively embedded to form a sliding connection; the lower ends of the support columns 321 are provided with a plurality of limit slots 320; the front ends of the four step-by-step discharge plates 33 are provided with handles; The rear end of the step-by-step discharge plate is provided with a wedge 330 which is inserted into the limiting groove 320; the four step-by-step discharge plates 33 are provided with four positioning pin holes 331 at intervals; the four guide bins 32 The sides are provided with sliding pins 323 which are vertically downward and match with the four positioning pin holes 331 .
这种技术方案的优势在于:首先配料桶31具备四个导料仓32,可实现预先分配储存生物陶瓷-可降解高分子混合粉末,方便进行不同物料的初步混料处理;支撑柱321用于连接四个导料仓32的侧壁,保证固定更加稳定;在进行配料导入时,四个定位销孔可看做每个导料仓排料量的大小档位,即需要投入比例更多导料仓,可将分阶排料板最大限度抽出,让滑动插销323插入分阶排料板最右端的定位销孔,即可拉开一个让物料导出的最大空间,即通过滑动插销与每一个定位销孔的固定,来控制该导料仓流出物料的量;通过在四个不同导料仓中进行不同的上述配置,就可以在四个导料仓中形成导出物料的不同混合比例,实现一种物料混合比例调整的功能,所混合的物料可统一排料管322向下排出,完成了混合物料的统一排出功能。The advantages of this technical solution are: firstly, the batching
在上述技术方案中,所述配料桶31中设置有振动架34;所述支撑柱为中空结构;所述振动架34中部设置有一根活动穿设在支撑柱321内部的滑杆341;所述支撑柱321两端设置有直线轴承342;所述滑杆341上端固定设置在其中一个直线轴承342的内圈上,且穿出后固定设置有翻料架35;所述翻料架35上端固定连接有直线往复电机350的输出端;所述翻料架35包括四个分别伸入到四个导料仓32中的翻料杆351;四个所述翻料杆351上间隔设置有多个斜杆352;多个所述斜杆352上分别横向设置有多个翻料片353;所述滑杆341下端固定设置在另外一个直线轴承342的内圈上,且穿出后固定设置有匀料台36;所述匀料台36悬空穿设于排料管322中;所述匀料台36上设置有十字结构的翻料爪361;四个所述翻料爪361上端分别设置有两个向中抵靠的弧面362;In the above technical solution, a vibrating
这种技术方案的优势在于:The advantages of this technical solution are:
(1)通过使用一种复合结构的振动架34,一起对四个导料仓32内部的物料进行统一翻动;滑杆341作为一个滑动件,在中空的固定柱321中部滑动,通过两个直线轴承342进行稳定的上下往复运动,直线往复电机350提供了运动动力;四个翻料杆351在分别伸入导料仓32后,配合翻料杆351连同多个斜杆352上的翻料片353,进行上下稳定的循环翻料,保证物料能够稳定从下方均匀导出;(1) By using a vibrating
(2)振动架下方匀料台36也随着滑杆341上下抖动,让从四个方向汇聚而来的不同物料能够被打散,并混合为更为均匀的状态,再向下排出;同时匀料台上的四个翻料爪361进行不停的上下运动,能够防止汇聚在排料管322中的物料堆积,提高排料效率;两个向中抵靠的弧面362,保证颗粒状的物料能够滑动下落能力,提高整体排料效果。(2) The screeding table 36 under the vibrating frame also shakes up and down with the sliding
在上述技术方案中,还包括一个螺旋进料机30;所述螺旋进料机30的输出端对接至分段式机筒1的首段;所述配料桶31下端一体设置有锥形的排料漏斗311;所述螺旋进料机30的输入端对接至排料漏斗311的下端口;所述排料漏斗311的中部横向可滑动设置有推拉板37;所述排料漏斗311侧面贯穿设置有条形的滑动架;所述滑动架两侧设置有滑槽Ⅱ;所述推拉板37两侧设置有可分别嵌入两个滑槽Ⅱ的滑条Ⅱ,从而实现了可滑动连接;所述推拉板37上设置有可与排料管322进行匹配对接的大、中、小限流口;所述中限流口372两侧设置有弹性挡板374;所述小限流口371和大下限流口373的一侧分别设置有固定挡板375。In the above technical solution, a
这种技术方案的优势在于:作业人员可通过不停滑动调整推拉板,来使得不同限流口对接至排料管322下端口,从而调整物料混料后的最终出料排量;两个弹性挡板374即可实现限位,保证中限流口372能够准确对接至排料管322下端口,同时在推拉板整体拖动时,弹性挡板能够被压缩,保证大限流口373和小限流口371都能滑动对接至排料管322的下端口,两个固定挡板能够初始端和最末端对滑动的推拉板实现整体的限位,使其更加稳定。The advantage of this technical solution is that the operator can adjust the push-pull plate by sliding continuously, so that the different restrictor ports are connected to the lower port of the
在上述技术方案中,所述挤出单元4包括:异向布置的大导程双螺杆41,其轴向可转动穿设在分段式机筒1中;所述双螺杆41外花键键齿410倾斜1°。In the above technical solution, the extrusion unit 4 includes: large-lead twin screws 41 arranged in opposite directions, which are axially rotatably penetrated in the segmented barrel 1; the twin screws 41 are externally splined. The
这种技术方案具备的优势在于:挤出单元4采用具有异向大导程螺纹结构的双螺杆41,实现了高分子熔体的周向流动和物料交换,克服了热敏性高分子长时间停留降解与塑化混合不充分的拮抗难题;同时,双螺杆外花键键齿倾斜1°,提出了渐开小角花键连接技术,保证了流道壁上剪切应力的稳定性,突破了流道内壁结垢和静态层形成的关键技术瓶颈。The advantage of this technical solution is that the extrusion unit 4 adopts a
在上述技术方案中,还包括动力单元;所述动力单元包括:进料电机51和主轴电机52;所述进料电机51设置在进料单元3前方,所述主轴电机52设置在分段式机筒1前方,通过一个变速箱53与双螺杆41连接。In the above technical solution, a power unit is also included; the power unit includes: a feeding
这种技术方案具备的优势在于:动力单元5所配置的进料电机51和主轴电机52为为挤出单元和进料单元的相关运转设备提供了稳定可控的动力能源,配置方便,物料挤出更加稳定。The advantages of this technical solution are: the feeding
在上述技术方案中,还包括加热单元;所述加热单元包括:电磁阀、加热器、温控表;所述加热器61具有多个,且分别设置在多个加热机筒11中。In the above technical solution, a heating unit is also included; the heating unit includes: a solenoid valve, a heater, and a temperature control meter; there are multiple heaters 61 and are respectively arranged in the multiple heating cylinders 11 .
这种技术方案的优点在于:通过加热单元中的个设备,为加热机筒提供了加热能力,配置方便,加热温度容易调控。The advantages of this technical solution are: the heating capacity is provided for the heating barrel through the equipment in the heating unit, the configuration is convenient, and the heating temperature is easy to control.
在上述技术方案中,还包括保护单元;所述保护单元包括:进气管71、增压泵72、出气管73、氮气罐74;所述增压泵72输入端通过出气管73连接氮气罐74;所述增压泵72输出端通过出气管73连接至分段式机筒1的首段。In the above technical solution, a protection unit is also included; the protection unit includes: an inlet pipe 71, a booster pump 72, an outlet pipe 73, and a nitrogen tank 74; the input end of the booster pump 72 is connected to the nitrogen tank 74 through the gas outlet pipe 73. ; The output end of the booster pump 72 is connected to the first section of the segmented barrel 1 through the air outlet pipe 73 .
这种技术方案的优点在于:保护单元的各个设备组成了一个增压式氮气注入保护系统,在生物陶瓷-可降解高分子混合粉末的熔融挤出过程中,不断导入氮气进行配合作业,能够有效防止了高温环境下生物陶瓷-可降解高分子混合粉末的热氧降解,提高物料热熔混料的制备品质。The advantage of this technical solution is that each equipment of the protection unit forms a pressurized nitrogen injection protection system. During the melt extrusion process of the bioceramic-degradable polymer mixed powder, nitrogen is continuously introduced for cooperation, which can effectively The thermo-oxidative degradation of the bioceramic-degradable polymer mixed powder in a high temperature environment is prevented, and the preparation quality of the material hot-melt mixture is improved.
在上述技术方案中,还包括操作单元;所述操作单元包括一个固定设置于分段式机筒1一侧的操控架81;所述操控架81上设置有显示操控屏82。In the above technical solution, an operation unit is also included; the operation unit includes a control frame 81 fixedly arranged on one side of the segmented barrel 1 ; the control frame 81 is provided with a display control screen 82 .
这种技术方案的优点在于:方便作业人员能够及时通过操控显示操控屏82来控制相关作业设备,控制方便,参数调整及时。The advantages of this technical solution are: it is convenient for the operator to control the relevant operation equipment by manipulating the display control screen 82 in time, the control is convenient, and the parameter adjustment is timely.
这里说明的设备数量和处理规模是用来简化本发明的说明的。对本发明的应用、修改和变化对本领域的技术人员来说是显而易见的。The number of apparatuses and processing scales described here are intended to simplify the description of the present invention. Applications, modifications and variations to the present invention will be apparent to those skilled in the art.
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节和这里示出与描述的图例。Although the embodiment of the present invention has been disclosed as above, it is not limited to the application listed in the description and the embodiment, and it can be applied to various fields suitable for the present invention. For those skilled in the art, it can be easily Therefore, the invention is not limited to the specific details and illustrations shown and described herein without departing from the general concept defined by the appended claims and the scope of equivalents.
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