CN108148011A - High melamine polyphosphate of a kind of thermal stability and preparation method thereof - Google Patents
High melamine polyphosphate of a kind of thermal stability and preparation method thereof Download PDFInfo
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 64
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229920000388 Polyphosphate Polymers 0.000 title claims abstract description 52
- 239000001205 polyphosphate Substances 0.000 title claims abstract description 52
- 235000011176 polyphosphates Nutrition 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 30
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 5
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 5
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000008240 homogeneous mixture Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 6
- 239000003063 flame retardant Substances 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
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Abstract
本发明公开了一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，其包括以下步骤：a.向三聚氰胺加入水，开启搅拌，继续滴入磷酸后反应1h即得三聚氰胺磷酸盐；b.将步骤a得到的三聚氰胺磷酸盐和处理剂混合均匀得到混匀物，所述处理剂选自尿素、碳酸氢铵或缩二脲中的一种或几种；c.将步骤b得到的混匀物在180‑260℃下进行热处理，热处理完成后冷却，即得到本发明中所述热稳定性高的三聚氰胺聚磷酸盐。按照本发明提供的制备方法最终得到的三聚氰胺聚磷酸盐的聚合度较高、水溶性降低、热稳定性优异，亦不会出现颜色变化，本发明提供的制备方法中热处理的温度和现有技术相比显著降低，降低了生产能耗，具有极为广阔的应用前景。The invention discloses a preparation method of melamine polyphosphate with high thermal stability, which comprises the following steps: a. adding water to melamine, starting stirring, continuing to drip phosphoric acid and reacting for 1 hour to obtain melamine phosphate; b. The melamine phosphate obtained in step a and the treatment agent are mixed uniformly to obtain a mixture, and the treatment agent is selected from one or more of urea, ammonium bicarbonate or biuret; c. the mixture obtained in step b Carry out heat treatment at 180-260° C., and cool after heat treatment to obtain the melamine polyphosphate with high thermal stability described in the present invention. According to the preparation method provided by the present invention, the melamine polyphosphate finally obtained has a high degree of polymerization, reduced water solubility, excellent thermal stability, and no color change. The temperature of heat treatment in the preparation method provided by the present invention and the prior art Significantly lower compared to the production energy consumption, has a very broad application prospects.
Description
技术领域technical field
本发明涉及三聚氰胺聚磷酸盐的制备，特别涉及到一种热稳定性高的三聚氰胺聚磷酸盐及其制备方法。The invention relates to the preparation of melamine polyphosphate, in particular to a melamine polyphosphate with high thermal stability and a preparation method thereof.
背景技术Background technique
随着阻燃材料的广泛应用，以及人们对环境保护的重视，环保型阻燃剂的开发也越来越备受关注，作为无卤环保型阻燃剂的代表，三聚氰胺聚磷酸盐（MPP）也成为了人们研究和开发的热点，该阻燃剂几乎可用于所有塑料，尤其适用于加工温度较高的工程塑料阻燃，如玻纤增强型尼龙、聚酯等高分子材料。With the wide application of flame retardant materials and people's emphasis on environmental protection, the development of environmentally friendly flame retardants has attracted more and more attention. As a representative of halogen-free environmentally friendly flame retardants, melamine polyphosphate (MPP) It has also become a hot spot of research and development. The flame retardant can be used in almost all plastics, especially for engineering plastics with high processing temperature, such as glass fiber reinforced nylon, polyester and other polymer materials.
目前，制备三聚氰胺聚磷酸盐的方法通常可分为一步法和两步法。一步法采用三聚氰胺与聚磷酸在一定条件下反应一步合成，但该方法受到聚磷酸的强吸水性和水解性的影响，使得其操作条件苛刻，目标产物成分复杂，其产品纯度偏低，制备得到的三聚氰胺聚磷酸盐效果明显劣于两步法。两步法是先三聚氰胺与磷酸反应合成中间体，然后再经过热处理制得三聚氰胺聚磷酸盐。据实际生产经验，必须要将中间产物在320℃以上的高温热处理一段时间以后，才能生产出热稳定性较高的三聚氰胺聚磷酸盐，而在如此高的温度下进行热处理的缺陷也较为明显，首先，经过高温下热处理得带的最终产物三聚氰胺聚磷酸盐的热稳定性虽然相对于中间产物有了一定程度上的提高，但是经热重分析法测试后，发现失重1%时，其分解温度低于360℃，热稳定性仍然需要进一步提高；其次，温度过高会导致最终得到的三聚氰胺聚磷酸盐的颜色出现土黄色，限制了其在浅色塑料中的应用；另外，高温下热处理还将导致能源的浪费，增加生产成本。At present, the method for preparing melamine polyphosphate can generally be divided into one-step method and two-step method. The one-step method uses melamine and polyphosphoric acid to react in one step under certain conditions, but this method is affected by the strong water absorption and hydrolysis of polyphosphoric acid, which makes its operating conditions harsh, the target product has complex components, and its product purity is low. The effect of melamine polyphosphate was significantly worse than that of the two-step method. The two-step method is to firstly react melamine and phosphoric acid to synthesize an intermediate, and then undergo heat treatment to obtain melamine polyphosphate. According to actual production experience, the intermediate product must be heat-treated at a high temperature above 320°C for a period of time before the melamine polyphosphate with high thermal stability can be produced, and the defects of heat treatment at such a high temperature are also obvious. First of all, although the thermal stability of the final product melamine polyphosphate obtained by heat treatment at high temperature has been improved to a certain extent compared with the intermediate product, after the test by thermogravimetric analysis, it was found that when the weight loss was 1%, the decomposition temperature If the temperature is lower than 360°C, the thermal stability still needs to be further improved; secondly, if the temperature is too high, the color of the final melamine polyphosphate will appear khaki, which limits its application in light-colored plastics; Will lead to waste of energy and increase production costs.
发明内容Contents of the invention
本发明要解决的技术问题在于提供一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，使用该制备方法可有效降低生产能耗，节约生产成本。The technical problem to be solved by the present invention is to provide a preparation method of melamine polyphosphate with high thermal stability, which can effectively reduce production energy consumption and save production cost.
为了解决上述技术问题，本发明采用以下技术方案：一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，包括以下步骤：In order to solve the problems of the technologies described above, the present invention adopts the following technical scheme: a kind of preparation method of melamine polyphosphate with high thermal stability comprises the following steps:
a.向三聚氰胺加入水，开启搅拌，继续滴入磷酸后反应1h即得三聚氰胺磷酸盐；a. Add water to melamine, start stirring, continue dropping phosphoric acid and react for 1 hour to obtain melamine phosphate;
b.将步骤a得到的三聚氰胺磷酸盐和处理剂混合均匀得到混匀物，所述处理剂选自尿素、碳酸氢铵或缩二脲中的一种或几种；b. mix the melamine phosphate obtained in step a and the treatment agent to obtain a homogeneous mixture, and the treatment agent is selected from one or more of urea, ammonium bicarbonate or biuret;
c.将步骤b得到的混匀物在180-260℃下进行热处理，热处理完成后冷却，即得到本发明中所述热稳定性高的三聚氰胺聚磷酸盐。c. heat-treat the mixture obtained in step b at 180-260° C., and cool after the heat treatment to obtain the melamine polyphosphate with high thermal stability described in the present invention.
优选地，步骤a中所述三聚氰胺与磷酸的质量比为5:2-5:4。Preferably, the mass ratio of melamine to phosphoric acid in step a is 5:2-5:4.
优选地，步骤a滴入磷酸反应1h后进行过滤、洗涤、干燥处理。Preferably, in step a, phosphoric acid is added dropwise and reacted for 1 hour, followed by filtering, washing and drying.
更优选地，所述干燥在真空条件下进行，干燥温度为130℃-140℃，干燥时间为2h-3h。More preferably, the drying is carried out under vacuum conditions, the drying temperature is 130°C-140°C, and the drying time is 2h-3h.
优选地，步骤b中所述三聚氰胺磷酸盐和所述处理剂之间的质量比为1:0.01-1:0.30。Preferably, the mass ratio between the melamine phosphate and the treatment agent in step b is 1:0.01-1:0.30.
优选地，步骤c中所述热处理的温度为180℃-230℃。Preferably, the temperature of the heat treatment in step c is 180°C-230°C.
优选地，步骤c中所述热处理的时间为1h-5h 。Preferably, the heat treatment time in step c is 1h-5h.
一种热稳定性高的三聚氰胺聚磷酸盐，由上述制备方法制备得到。A melamine polyphosphate with high thermal stability is prepared by the above preparation method.
和现有技术相比，本发明具有以下有益效果：本发明首先通过将三聚氰胺和磷酸反应得到三聚氰胺磷酸盐，然后向三聚氰胺磷酸盐加入特定的处理剂（尿素、碳酸氢铵或缩二脲中的一种或几种），并在特定的温度范围180℃-260℃内进行热处理，最终得到的三聚氰胺聚磷酸盐的聚合度较高、水溶性降低、热稳定性优异，检测后发现该最终得到的三聚氰胺聚磷酸盐失重1%的温度大于380℃，由于本发明中对中间产物三聚氰胺磷酸盐进行热处理的温度很低，不仅防止了最终产物三聚氰胺聚磷酸盐由于温度过高变为土黄色，而且降低了生产能耗，节约了成本，具有极为广阔的应用前景。Compared with the prior art, the present invention has the following beneficial effects: the present invention at first obtains melamine phosphate by reacting melamine and phosphoric acid, then adds specific treatment agent (in urea, ammonium bicarbonate or biuret) to melamine phosphate One or several) and heat treatment in a specific temperature range of 180°C-260°C, the final melamine polyphosphate has a higher degree of polymerization, reduced water solubility, and excellent thermal stability. After testing, it was found that the final melamine polyphosphate The temperature of melamine polyphosphate weight loss 1% is greater than 380 ℃, because the temperature that intermediate product melamine phosphate is heat-treated in the present invention is very low, not only has prevented final product melamine polyphosphate from becoming earthy yellow because temperature is too high, and The production energy consumption is reduced, the cost is saved, and the method has extremely broad application prospects.
具体实施方式Detailed ways
下面给出实施例以对本发明进行具体的描述，有必要在此指出的是以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的普通技术人员根据该实施例对本发明所做出的一些非本质的改进或调整仍属于本发明的保护范围。The following examples are provided below to specifically describe the present invention. It is necessary to point out that the following examples are only used to further illustrate the present invention, and cannot be interpreted as limiting the protection scope of the present invention. Some non-essential improvements or adjustments made by the embodiments to the present invention still belong to the protection scope of the present invention.
实施例1Example 1
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，包括以下步骤：A kind of preparation method of the high thermal stability melamine polyphosphate, comprises the following steps:
a.称取25.2g三聚氰胺，置于装有电动搅拌器、温度计、恒压滴液漏斗的1000mL四口烧瓶中，向四口烧瓶中加入蒸馏水600mL，并搅拌，在常温下，通过恒压滴液漏斗缓慢滴入23.1g质量浓度为85%的磷酸溶液，约1小时滴加完成，待磷酸溶液滴加完成，继续反应1小时，过滤，洗涤，于130℃下真空干燥3小时，得43.5g 三聚氰胺磷酸盐；a. Weigh 25.2g of melamine, place it in a 1000mL four-necked flask equipped with an electric stirrer, a thermometer, and a constant pressure dropping funnel, add 600mL of distilled water to the four-necked flask, and stir. Slowly drop 23.1 g of phosphoric acid solution with a mass concentration of 85% into the liquid funnel, and the dropwise addition is completed in about 1 hour. After the addition of the phosphoric acid solution is completed, continue the reaction for 1 hour, filter, wash, and vacuum dry at 130 ° C for 3 hours to obtain 43.5 g melamine phosphate;
b.将步骤a得到的三聚氰胺磷酸盐粉碎，加入尿素4 g并混合均匀得到混匀物；b. pulverize the melamine phosphate obtained in step a, add 4 g of urea and mix uniformly to obtain a mixture;
c.将步骤b得到的混匀物在260℃下热处理1小时，冷却，即得到产品三聚氰胺聚磷酸盐38.2 g。c. heat-treat the mixture obtained in step b at 260° C. for 1 hour, and cool to obtain 38.2 g of the product melamine polyphosphate.
实施例2Example 2
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，包括以下步骤：A kind of preparation method of the high thermal stability melamine polyphosphate, comprises the following steps:
a.称取25.2g三聚氰胺，置于装有电动搅拌器、温度计和恒压滴液漏斗的1000mL四口烧瓶中，向四口烧瓶中加入600mL水并搅拌，在常温下，通过恒压滴液漏斗缓慢滴入18.4g质量浓度为85%磷酸溶液 ，待磷酸溶液滴加完成，待磷酸溶液滴加完成，继续反应1小时，过滤，洗涤，于130℃下真空干燥2小时，得40.9g 三聚氰胺磷酸盐；a. Weigh 25.2g of melamine, place it in a 1000mL four-necked flask equipped with an electric stirrer, a thermometer and a constant pressure dropping funnel, add 600mL of water to the four-necked flask and stir, at room temperature, through constant pressure dropping Slowly drop 18.4g of phosphoric acid solution with a mass concentration of 85% into the funnel. After the addition of phosphoric acid solution is completed, continue to react for 1 hour, filter, wash, and vacuum dry at 130°C for 2 hours to obtain 40.9g of melamine. Phosphate;
b.将步骤a得到的三聚氰胺磷酸盐粉碎，加入碳酸氢铵5.3g并混合均匀得到混匀物；b. pulverize the melamine phosphate obtained in step a, add 5.3 g of ammonium bicarbonate and mix uniformly to obtain a blend;
c.将步骤b得到的混匀物在180℃下热处理5小时，冷却，即得到产品三聚氰胺聚磷酸盐32.1g。c. heat-treat the mixture obtained in step b at 180° C. for 5 hours, and cool to obtain 32.1 g of the product melamine polyphosphate.
实施例3Example 3
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，包括以下步骤：A kind of preparation method of the high thermal stability melamine polyphosphate, comprises the following steps:
a.称取25.2g三聚氰胺，置于装有电动搅拌器、温度计和恒压滴液漏斗的1000mL四口烧瓶中，向四口烧瓶中加入600mL水并搅拌，在常温下，通过恒压滴液漏斗缓慢滴入13.8g质量浓度为85%的磷酸溶液，待磷酸溶液滴加完成，继续反应1小时，过滤，洗涤，于130℃下真空干燥2小时，得35.4g 三聚氰胺磷酸盐；a. Weigh 25.2g of melamine, place it in a 1000mL four-necked flask equipped with an electric stirrer, a thermometer and a constant pressure dropping funnel, add 600mL of water to the four-necked flask and stir, at room temperature, through constant pressure dropping Slowly drop 13.8 g of phosphoric acid solution with a mass concentration of 85% into the funnel. After the phosphoric acid solution is added dropwise, continue the reaction for 1 hour, filter, wash, and vacuum dry at 130 ° C for 2 hours to obtain 35.4 g of melamine phosphate;
b.将步骤a得到的三聚氰胺磷酸盐粉碎，加入缩二脲6.0g并混合均匀得到混匀物；b. Pulverize the melamine phosphate obtained in step a, add 6.0 g of biuret and mix evenly to obtain a blend;
c.将步骤b得到的混匀物在230℃下热处理3小时，冷却，即得到产品三聚氰胺聚磷酸盐25.6 g。c. heat-treat the mixture obtained in step b at 230° C. for 3 hours, and cool to obtain 25.6 g of the product melamine polyphosphate.
对比例1Comparative example 1
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，和实施例1相比，唯一区别为省去了步骤b，即将步骤a中得到的三聚氰胺磷酸盐直接进行步骤c中的热处理、冷却即得产品三聚氰胺聚磷酸盐。A method for preparing melamine polyphosphate with high thermal stability, compared with Example 1, the only difference is that step b is omitted, that is, the melamine phosphate obtained in step a is directly subjected to heat treatment and cooling in step c. The product melamine polyphosphate is obtained.
对比例2Comparative example 2
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，和实施例2比，唯一区别为省去了步骤b，即将步骤a中得到的三聚氰胺磷酸直接进行步骤c中的热处理、冷却即得产品三聚氰胺聚磷酸盐。A method for preparing melamine polyphosphate with high thermal stability. Compared with Example 2, the only difference is that step b is omitted, that is, the melamine phosphoric acid obtained in step a is directly subjected to heat treatment and cooling in step c to obtain the product Melamine polyphosphate.
对比例3Comparative example 3
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，和实施例3比，唯一区别为省去了步骤b，即将步骤a中得到的三聚氰胺磷酸直接进行步骤c中的热处理、冷却即得产品三聚氰胺聚磷酸盐。A method for preparing melamine polyphosphate with high thermal stability. Compared with Example 3, the only difference is that step b is omitted, that is, the melamine phosphoric acid obtained in step a is directly subjected to heat treatment and cooling in step c to obtain the product Melamine polyphosphate.
对比例4Comparative example 4
一种热稳定性高的三聚氰胺聚磷酸盐的制备方法，和实施例2比，唯一区别为将步骤c中的热处理温度由180℃改为320℃，其他均与实施例2保持一致。A method for preparing melamine polyphosphate with high thermal stability. Compared with Example 2, the only difference is that the heat treatment temperature in step c is changed from 180°C to 320°C, and the others are consistent with Example 2.
性能数据测试方法Performance Data Test Method
热稳定性测试：采用热重分析法，即分别取实施例1-3和对比例1-4中得到的少量三聚氰胺磷酸盐和产品三聚氰胺聚磷酸盐作为样品，以热天平作为测试仪器，将样品加热，样品受热后重量变化引起天平位移量转化成电磁量，这个微小的电量经过放大器放大后，送入记录仪记录，而电量的大小正比于样品的重量变化量。当被测物质在加热过程中出现重量变化时，热重曲线就会有所下降，通过分析热重曲线，就可以知道被测样品在多少度时发生多大重量的变化，本发明中的具体实施方式中测试的是样品重量减少1%时的温度大小。Thermal stability test: adopt thermogravimetric analysis, promptly take a small amount of melamine phosphate obtained in embodiment 1-3 and comparative example 1-4 and product melamine polyphosphate as sample respectively, take thermobalance as testing instrument, sample Heating, the weight change of the sample after heating causes the balance displacement to be converted into electromagnetic quantity. After the tiny electric quantity is amplified by the amplifier, it is sent to the recorder for recording, and the electric quantity is proportional to the weight change of the sample. When the weight of the measured substance changes during the heating process, the thermogravimetric curve will drop. By analyzing the thermogravimetric curve, it can be known how much weight changes the tested sample occurs at what degree. The specific implementation of the present invention What is tested in the method is the temperature when the sample weight is reduced by 1%.
水溶性测试：将取实施例1-3和对比例1-4中的少量产品三聚氰胺聚磷酸盐作为样品，加入重量为样品49倍的水中得到2wt%的浆液，然后测试该浆液中三聚氰胺聚磷酸盐的溶解度。Water Solubility Test: A small amount of product melamine polyphosphate in Examples 1-3 and Comparative Examples 1-4 will be taken as a sample, and a 2wt% slurry will be obtained by adding 49 times the weight of the sample, and then the melamine polyphosphate in the slurry will be tested Salt solubility.
实施例1-3和对比例1-4中三聚氰胺磷酸盐和产品三聚氰胺聚磷酸盐的性能参数测试结果见下表1所示。The test results of performance parameters of melamine phosphate and product melamine polyphosphate in Examples 1-3 and Comparative Examples 1-4 are shown in Table 1 below.
由表1可知，利用本发明提供的方法制备得到的三聚氰胺聚磷酸盐通过热重分析法测试后，发现该三聚氰胺聚磷酸盐失重1%温度可达到380℃以上，其在水中的溶解度在0.016g/100mL以下，即本发明中最终制备得到的三聚氰胺聚磷酸盐的热稳定性较好，水溶性较低，而对比例1-3由于对三聚氰胺磷酸盐在180℃-260℃条件下进行热处理之前未加入处理剂，导致最终制备得到的产品三聚氰胺聚磷酸盐失重1%温度相对于步骤a中得到的三聚氰胺磷酸盐并无提高，且溶解度劣于实施例1-3。As can be seen from Table 1, after the melamine polyphosphate prepared by the method provided by the present invention is tested by thermogravimetric analysis, it is found that the temperature of 1% weight loss of the melamine polyphosphate can reach above 380°C, and its solubility in water is 0.016g /100mL or less, that is, the thermal stability of the melamine polyphosphate finally prepared in the present invention is better, and the water solubility is lower, and the comparative example 1-3 is due to the melamine phosphate before heat treatment under the condition of 180°C-260°C No treatment agent was added, resulting in the 1% weight loss of the final product melamine polyphosphate. Compared with the melamine phosphate obtained in step a, the temperature did not increase, and the solubility was worse than that of Examples 1-3.
另外由表1中的对比例4和实施例2可知，由于对比例4的热处理温度过高，导致最终得到的三聚氰胺聚磷酸盐出现土黄色，其测试得到的热稳定性和水溶性也均劣于实施例2。In addition, as can be seen from Comparative Example 4 and Example 2 in Table 1, because the heat treatment temperature of Comparative Example 4 is too high, the melamine polyphosphate finally obtained is khaki, and the thermal stability and water solubility obtained by the test are also poor. In Example 2.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111285817A (en) * | 2020-04-07 | 2020-06-16 | 四川省精细化工研究设计院 | Melamine polyphosphate and application thereof |
| CN112431021A (en) * | 2020-11-24 | 2021-03-02 | 常州大学 | Preparation method of flame-retardant natural loofah sponge |
| RU2758253C1 (en) * | 2021-03-15 | 2021-10-27 | Федеральное государственное автономное образовательное учреждение высшего образования «Национальный исследовательский Томский государственный университет» | Method for obtaining melamine polyphosphate |
| CN116120250A (en) * | 2022-11-28 | 2023-05-16 | 安徽南都华铂新材料科技有限公司 | Method for preparing melamine phosphate and melamine polyphosphate from iron phosphate slag |
| CN117069948A (en) * | 2023-10-17 | 2023-11-17 | 四川省成都市福来隆科技有限公司 | Preparation method of melamine polyphosphate containing aldehyde functional group |
| CN117089079A (en) * | 2023-10-17 | 2023-11-21 | 四川省成都市福来隆科技有限公司 | Preparation method of melamine polyphosphate containing carboxyl functional groups |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL249727A1 (en) * | 1984-09-21 | 1986-03-25 | Inst Chemii Nieorganicznej | Method of obtaining melamine polyphosphate |
| JPH11246778A (en) * | 1998-03-04 | 1999-09-14 | Unitika Ltd | Flame retardant resin composition |
| CN102127230A (en) * | 2010-01-19 | 2011-07-20 | 中化蓝天集团有限公司 | New process for preparing modified melamine polyphosphate |
| CN104513210A (en) * | 2013-09-29 | 2015-04-15 | 青岛市首胜实业有限公司 | Preparation method for intumescent flame retardant melamine phosphate |
| CN105504292A (en) * | 2015-12-24 | 2016-04-20 | 瓮福（集团）有限责任公司 | Preparation method of MPOP |
| CN105924651A (en) * | 2016-05-09 | 2016-09-07 | 东华大学 | Preparation method of high-polymerization-degree melamine polyphosphate |
-
2018
- 2018-01-18 CN CN201810048963.7A patent/CN108148011A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL249727A1 (en) * | 1984-09-21 | 1986-03-25 | Inst Chemii Nieorganicznej | Method of obtaining melamine polyphosphate |
| JPH11246778A (en) * | 1998-03-04 | 1999-09-14 | Unitika Ltd | Flame retardant resin composition |
| CN102127230A (en) * | 2010-01-19 | 2011-07-20 | 中化蓝天集团有限公司 | New process for preparing modified melamine polyphosphate |
| CN104513210A (en) * | 2013-09-29 | 2015-04-15 | 青岛市首胜实业有限公司 | Preparation method for intumescent flame retardant melamine phosphate |
| CN105504292A (en) * | 2015-12-24 | 2016-04-20 | 瓮福（集团）有限责任公司 | Preparation method of MPOP |
| CN105924651A (en) * | 2016-05-09 | 2016-09-07 | 东华大学 | Preparation method of high-polymerization-degree melamine polyphosphate |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111285817A (en) * | 2020-04-07 | 2020-06-16 | 四川省精细化工研究设计院 | Melamine polyphosphate and application thereof |
| CN112431021A (en) * | 2020-11-24 | 2021-03-02 | 常州大学 | Preparation method of flame-retardant natural loofah sponge |
| RU2758253C1 (en) * | 2021-03-15 | 2021-10-27 | Федеральное государственное автономное образовательное учреждение высшего образования «Национальный исследовательский Томский государственный университет» | Method for obtaining melamine polyphosphate |
| CN116120250A (en) * | 2022-11-28 | 2023-05-16 | 安徽南都华铂新材料科技有限公司 | Method for preparing melamine phosphate and melamine polyphosphate from iron phosphate slag |
| CN117069948A (en) * | 2023-10-17 | 2023-11-17 | 四川省成都市福来隆科技有限公司 | Preparation method of melamine polyphosphate containing aldehyde functional group |
| CN117089079A (en) * | 2023-10-17 | 2023-11-21 | 四川省成都市福来隆科技有限公司 | Preparation method of melamine polyphosphate containing carboxyl functional groups |
| CN117089079B (en) * | 2023-10-17 | 2023-12-26 | 四川省成都市福来隆科技有限公司 | Preparation method of melamine polyphosphate |
| CN117069948B (en) * | 2023-10-17 | 2024-01-02 | 四川省成都市福来隆科技有限公司 | Preparation method of melamine polyphosphate containing aldehyde functional group |
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