CN106565907A - Preparation method for nanocellulose enhanced bio-based nano rubber latex - Google Patents
Preparation method for nanocellulose enhanced bio-based nano rubber latex Download PDFInfo
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- CN106565907A CN106565907A CN201610972738.3A CN201610972738A CN106565907A CN 106565907 A CN106565907 A CN 106565907A CN 201610972738 A CN201610972738 A CN 201610972738A CN 106565907 A CN106565907 A CN 106565907A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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Abstract
The invention discloses a preparation method for nanocellulose enhanced bio-based nano rubber latex. The method comprises the steps of firstly performing enzymolysis, chemical oxidation pre-treatment and mechanical treatment on starch and plant cellulose fibers as raw materials to obtain nanocrystalline starch and nanocellulose; secondly mixing the nanocrystalline starch and the nanocellulose with natural non-grain degraded starch to prepare a uniform dispersed mixed solution, and performing activation modification treatment; thirdly adding an initiator to the mixed solution for initiating an emulsion polymerization reaction of double-bond monomers, and finally preparing a nanocellulose, nanocrystalline starch and non-grain degraded starch grafted copolymer, namely, the nanocellulose enhanced bio-based nano rubber latex. The nanocellulose and the nanocrystalline starch contained in the bio-based nano rubber latex achieve a remarkable enhancement effect for adhesion of rubber latex; and the bio-based nano rubber latex has the advantages of environmental protection, safety, sustainability and the like, and can be widely applied to the fields of papermaking, spinning, packaging, daily chemicals, building materials and the like.
Description
Technical field
The present invention relates to a kind of preparation method of nano-cellulose enhancement mode bio-based nano rubber latex, belongs to Chemical Engineering Technology neck
Domain.
Background technology
Adhesive refers to sticking and cohesion grade effect by interface, connects can two or more product or material
Natural or synthesis, the organic or inorganic class material being connected together, is referred to as adhesive, is called adhesive.According to
The source of adhesive can be divided into natural glue and synthetic adhesive, such as natural rubber, Colophonium, Colophonium, gelatin, fiber
Element, amylan etc. belong to natural glue, and belong to synthetic adhesive using the various adhesives of polymerization synthetic
Category.Wherein, the raw material great majority that synthetic adhesive is adopted are fossil class resources.
Into 21 century since, because of exploitation, the environmental pollution, greenhouse gas emission, the resource that are caused using fossil class resource
Exhausted the problems such as, increasingly highlights, and causes the highest attention and demand of whole world national governments and the people.Meanwhile, with the amount of containing
Source is abundant, inexpensive, renewable, green, eco-friendly natural biomass resource, partially or completely replaces fossil class resource,
Industrial quarters and scientific circles' joint research, the lasting focus of exploitation and focus are become.In adhesive industry, although synthetic adhesive
Production and application still occupy most ratios, but with the continuous development of science and technology, new, excellent performance, ring
The friendly all kinds of natural glues in border are flourished.
At present, some biological (starch base) latex products for occurring on market, although environmentally friendly and cheap, but generally deposit
Adhesion strength is low, not water-fast, easy aged deterioration, stability difference the shortcomings of, limit it to petroleum base synthetic adhesive
The lifting of substitution ratio.
The content of the invention
The present invention is for current synthetic adhesive, the shortcoming of common biology latex products and deficiency, there is provided a kind of Nanowire
The preparation method of the plain enhancement mode bio-based nano rubber latex of dimension.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of nano-cellulose enhancement mode bio-based nano rubber latex, comprises the following steps：
(1) with starch, Plant fiber's cellulose fiber as raw material, respectively by enzymolysis, chemical oxidation pre-treatment and machinery at
Reason, prepares nanocrystalline starch and nano-cellulose；
(2) the nanocrystalline starch of step (1) preparation, nano-cellulose are mixed with natural non-grain degradable starch, is made into
Even dispersion, then carries out activation modification process；Finally again emulsion polymerization is carried out to the dispersion after activation modification process anti-
Should, nano-cellulose, nanocrystalline starch and non-grain degradable starch emulsion graft copolymer, i.e. nano-cellulose is finally obtained to be strengthened
Type bio-based nano rubber latex.
Further, the preparation method of above-mentioned nano-cellulose enhancement mode bio-based nano rubber latex, wherein, described shallow lake
Powder is one or more in corn starch, tapioca, potato starch, rice starch.
Further, the preparation method of above-mentioned nano-cellulose enhancement mode bio-based nano rubber latex, wherein, described plant
Fibres cellulose fiber is one or more in lumber fibre, grass fiber, cotton fiber, flaxen fiber, pulp fibers.
Further, the preparation method of above-mentioned nano-cellulose enhancement mode bio-based nano rubber latex, wherein, step (1)
Described in enzymolysis processing, using compound cellulase, it contains endoglucanase (EG), exoglucanase (CBH), fiber
Plain disaccharidase (BG)；Enzymolysis processing technique is：First, water is added in retort；Then, weigh starch and fibrous raw material is added
To in retort, the mixed liquor of 1～10% concentration, moderate-speed mixer are made into；Then, the composite fibre of 1.0～10.0FPU/g is added
Plain enzyme, add buffer solution control mixed liquor reaction system pH value be 5.0 ± 0.2, control the temperature of reaction system be 40～
60 DEG C, the response time is 1～3h.Starch, the absolute dry mass ratio of Plant fiber's cellulose fiber are (1～30):1.
Further, the preparation method of above-mentioned nano-cellulose enhancement mode bio-based nano rubber latex, it is characterised in that：Step
Suddenly chemical oxidation pre-treatment described in (1), is additionization in the reaction system after starch, plant cellulose fiber enzymolysis processing
Learn oxidising agent, make the starch after oxidation and Plant fiber's cellulose fiber mixed liquor carboxyl-content be at least up to 0.80mmol/g and
More than.
Further, the chemical oxidation treatment described in step (1), wherein, the chemical oxidation reagent is 2,2,6,6-
Tetramethyl piperidine nitrogen oxides, sodium bromide, sodium metaperiodate, sodium hypochlorite, sodium chlorite or hydrogen peroxide.
Further, the mechanical treatment described in step (1), be using high pressure homogenizer, grinding and crushing machine, sand mill,
One or more in ball mill, ultrasonic cell disruptor, to respectively through enzymolysis and chemical oxidation treatment starch and
Plant fiber's cellulose fiber mixed liquor applies mechanism, obtains nanocrystalline starch and nano-cellulose with nano-scale；Its
In, the particle diameter of nanocrystalline starch is less than 100nm, and the fibril width of nano-cellulose is less than 100nm.
Further, in step (2), the over dry of starch and Plant fiber's cellulose fiber mixed liquor and natural non-grain degradable starch
Mass ratio is (1～10):100.
Further, activation modification described in step (2) process be etherified, be esterified, be crosslinked in one or more
Chemical modification process.
Further, the emulsion polymerization described in step (2) is added in the dispersion after activation modification process
Initiator, causes the emulsion polymerization of double bond class monomer.
Further, the performance indications that the nano-cellulose enhancement mode bio-based nano rubber latex described in step (2) has
For：50～100nm of particle diameter；Solid content 50 ± 2%；Viscosity≤500mPas；PH value 6.0-8.0；Mechanical stability (mass fraction)
≤ 0.03%；Coagulum content (mass fraction) (325 mesh)≤0.03%；40～55mN/m of surface tension；Vitrification point
(Tg) 10～50 DEG C.
The present invention has compared with prior art significant advantage and beneficial effect, embodies in the following areas：
1. it is of the invention by two kinds of biomass nano materials with unique enhancement effect：Nano-cellulose and nanocrystalline starch
Together with non-grain degradable starch, by way of emulsion graft copolymerization is closed, it is obtained and there is excellent high bonding force characteristic, nanoscale
The adhesive product of size, has the advantages that grease proofing high cohesive force, good film-forming property, water resistant, strong adaptability, with low cost；
2. synthetic adhesive-the carboxylic of the alternative Paper Coating of obtained nano-cellulose enhancement mode bio-based nano rubber latex
Base styrene-butadiene latex (SBR), substitution ratio reach 60% and more than, the IGT picking speed of coating paper (reflection adhesive it is viscous
Knot power) it is more than 2.0m/s, it is entirely capable of meeting the application requirement of Paper Coating High-performance adhesive；
3. raw material is from recyclable regenerative, biomass resource (Plant fiber, the starch of the nature amount of containing very abundant
Deng), biomass content is up to 90%, degradable, environmental protection, safe efficient；Not only can reduce the production of end product into
This, improves performance, improves the competitiveness of product, and the greenization of improving product, environmental protection can also be reduced to non-renewable change
The use of stone resource, reduces ambient pollution burden and carbon emission, to industrial structure optimization, transition and upgrade, social sustainable health
Development all tools are of great significance.
Specific embodiment
It is biological that the present invention prepares nano-cellulose enhancement mode using nanotechnology, zymolysis technique, emulsion polymerization technology research and development
Base nano rubber latex, belongs to new biomass nano material, can be attributed to natural glue category.It is that there is unique increasing by two kinds
The potent biomass nano material answered：Nano-cellulose and nanocrystalline starch together with non-grain degradable starch, by emulsion graft polymerization
The mode of combined polymerization, it is obtained a kind of with excellent high bonding force characteristic, nano-grade size adhesive product, with high viscous
Knot power, good film-forming property, grease proofing water resistant, strong adaptability, it is with low cost the advantages of.It is mainly used in papermaking, weaving, printing and bag
The effects such as the fields such as dress, daily use chemicals, building materials, medicine, electronic product, performance bonding, bonding, rheological characteristic improvement, machinery enhancing.Positioning
In to unsustainable, petroleum base synthetic adhesive vast scale replacement.
Embodiment 1：
Nanocrystalline starch and nano-cellulose are prepared first：The water of 2000g is added in the there-necked flask of 5000ml, is added
The broad-leaved wood fiber slurry that 40g original corn starchs, 20g have been crushed, is made into the dispersion that concentration is about 3%, and moderate-speed mixer is added
It is 5.0 ± 0.2 that buffer solution controls the pH value of dispersion, adds the compound cellulase of 2.0FPU/g, heating in water bath, reaction
Temperature 60 C, response time 2.5h.Then TEMPO is sequentially added in the dispersion, and (2,2,6,6- tetramethyl piperidines are aoxidized
Thing) 2.5g, sodium bromide 8.0g, liquor natrii hypochloritises 150g, with the sodium hydroxide solution of 10% concentration, control the oxidation reaction body
The pH value of system is 10.5,23 DEG C of reaction temperature, response time 1.5h.The carboxyl-content of starch and cellulose mixed liquor after oxidation
Reach 1.12mmol/g.Then mixed liquor is concentrated into 2.5% concentration, homogenizing is carried out to the concentration slurry with high pressure homogenizer
Change is processed, pressure 80MPa, circulation homogenizing 3 times, and the material of collection is mixing for nano-cellulose and nanocrystalline starch
Body.
The preparation of nano-cellulose enhancement mode bio-based nano rubber latex：In 200ml aqueous solutions, non-grain degradable starch is added
100g, the homogeneous mixture 10g, NaH of the nano-cellulose of above-mentioned preparation and nanocrystalline starch2PO47g, moderate-speed mixer, in 60
2h is reacted under DEG C water bath with thermostatic control, activation modification process is completed；5.0g emulsifying agent SDBS (dodecylbenzene sodium sulfonate) is added, is heated up
To 85 DEG C, then add 0.3g Ammonium persulfate .s as initiator in the mixed liquor, the acrylic acid of Deca 6.8g is added after 10min
Hydroxyl ethyl ester, while Deca 0.5g ammonium persulfate aqueous solution, 1h is added dropwise to complete, and is most cooled to 40 after 85 DEG C of insulation reaction 1h
DEG C, it is 6.5 to adjust pH value with ammonia, is discharged after stirring 30min, that is, obtain nano-cellulose enhancement mode bio-based nano rubber latex.
Embodiment 2：
Nanocrystalline starch and nano-cellulose are prepared first：The water of 2000g is added in the there-necked flask of 5000ml, is added
The cotton fiber slurry that 40g original corn starchs, 20g have been crushed, is made into the dispersion that concentration is about 2%, and moderate-speed mixer adds buffering
It is 5.0 ± 0.2 that solution controls the pH value of dispersion, adds the compound cellulase of 3.5FPU/g, heating in water bath, reaction temperature
60 DEG C, response time 3.5h.Then sodium metaperiodate 12.5g, sodium bicarbonate 5.0g are added in the dispersion, 2% concentration is used
Sodium hydroxide solution, control the oxidation reaction system pH value be 8.5,45 DEG C of reaction temperature, response time 2.5h.After oxidation
The carboxyl-content of starch and cellulose mixed liquor reach 1.35mmol/g.Then mixed liquor is concentrated into 2.5% concentration, is used
High pressure homogenizer carries out homogenize process to the concentration slurry, pressure 80MPa, circulation homogenizing 3 times, and the material of collection is nanometer
The homogeneous mixture of cellulose and nanocrystalline starch.
The preparation of nano-cellulose enhancement mode bio-based nano rubber latex：In 200ml aqueous solutions, non-grain degradable starch is added
100g, the homogeneous mixture 10g, NaH of the nano-cellulose of above-mentioned preparation and nanocrystalline starch2PO4 7g, moderate-speed mixer, in 60
2h is reacted under DEG C water bath with thermostatic control, activation modification process is completed；5.0g emulsifying agent SDBS (dodecylbenzene sodium sulfonate) is added, is heated up
To 85 DEG C, then add 0.3g Ammonium persulfate .s as initiator in the mixed liquor, the acrylic acid of Deca 6.8g is added after 10min
Hydroxyl ethyl ester, while Deca 0.5g ammonium persulfate aqueous solution, 1h is added dropwise to complete, and is most cooled to 40 after 85 DEG C of insulation reaction 1h
DEG C, it is 6.5 to adjust pH value with ammonia, is discharged after stirring 30min, that is, obtain nano-cellulose enhancement mode bio-based nano rubber latex.
Embodiment 3：
Nanocrystalline starch and nano-cellulose are prepared first：The water of 2000g is added in the there-necked flask of 5000ml, is added
The cotton fiber slurry that 40g original corn starchs, 20g have been crushed, is made into the dispersion that concentration is about 2%, and moderate-speed mixer adds buffering
It is 5.0 ± 0.2 that solution controls the pH value of dispersion, adds the compound cellulase of 3.5FPU/g, heating in water bath, reaction temperature
60 DEG C, response time 3.5h.Then sodium metaperiodate 12.5g, sodium bicarbonate 5.0g are added in the dispersion, 2% concentration is used
Sodium hydroxide solution, control the oxidation reaction system pH value be 8.5,45 DEG C of reaction temperature, response time 2.5h.After oxidation
The carboxyl-content of starch and cellulose mixed liquor reach 1.35mmol/g.Then mixed liquor is concentrated into 2.5% concentration, is used
High pressure homogenizer carries out homogenize process to the concentration slurry, pressure 80MPa, circulation homogenizing 3 times, and the material of collection is nanometer
The homogeneous mixture of cellulose and nanocrystalline starch.
The preparation of nano-cellulose enhancement mode bio-based nano rubber latex：In 200ml aqueous solutions, non-grain degradable starch is added
100g, homogeneous mixture 10g, the aluminate coupling agent 3.2g of the nano-cellulose of above-mentioned preparation and nanocrystalline starch, in 40 DEG C
2h is reacted under water bath with thermostatic control, activation modification process is completed；5.0g emulsifying agent SDBS (dodecylbenzene sodium sulfonate) is added, is warming up to
85 DEG C, then add 0.3g Ammonium persulfate .s as initiator in the mixed liquor, the metering system of Deca 4.5g is added after 10min
Allyl propionate, while Deca 1.3g ammonium persulfate aqueous solution, 1h is added dropwise to complete, and is most cooled to 40 after 80 DEG C of insulation reaction 1h
DEG C, it is 6.5 to adjust pH value with ammonia, is discharged after stirring 30min, that is, obtain nano-cellulose enhancement mode bio-based nano rubber latex.
The performance indications of above-mentioned nano-cellulose enhancement mode bio-based nano rubber latex are：50～100nm of particle diameter；Solid content 50
± 2%；Viscosity≤500mPas；PH value 6.0-8.0；Mechanical stability (mass fraction)≤0.03%；Coagulum content (quality
Fraction) (325 mesh)≤0.03%；40～55mN/m of surface tension；10～50 DEG C of vitrification point (Tg).
In sum, the obtained nano-cellulose enhancement mode bio-based nano rubber latex of the present invention is strong, biological with cohesive force
The advantages of matter content height, good, pollution-free being compatible with the environment property, applied range.The synthetic adhesive of alternative Paper Coating-
Carboxylic styrene butadiene latex (SBR), substitution ratio reach 60% and more than, the IGT picking speed of coating paper be (reflection adhesive
Cohesive force) it is more than 2.0m/s, it is entirely capable of meeting the application requirement of Paper Coating High-performance adhesive.
The raw material of nano-cellulose enhancement mode bio-based nano rubber latex from recyclable regenerative, the nature amount of containing very
Abundant biomass resource (Plant fiber, starch etc.), biomass content is up to 90%, degradable, environmental protection, safety, height
Effect.Using this new, high performance natural glue product, the production cost of end product not only can be reduced, be improved
Performance, improves the competitiveness of product, and the greenization of improving product, environmental protection can also be reduced to non-renewable fossil resource
Use, reduce the pollutional load and carbon emission of environment, to China's industrial structure optimization at this stage, transition and upgrade, society can
Sustainable and healthy development all has and is of great significance.
It should be noted that：The preferred embodiment of the present invention is the foregoing is only, the power of the present invention is not limited to
Sharp scope；Description more than simultaneously, for the special personage of correlative technology field should understand and implement, therefore other without departing from
The equivalent change completed under disclosed spirit or modification, in should be included in claim.
Claims (10)
1. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex, it is characterised in that：Comprise the following steps：
(1) with starch, Plant fiber's cellulose fiber as raw material, respectively by enzymolysis, chemical oxidation pre-treatment and mechanical treatment, system
It is standby to obtain nanocrystalline starch and nano-cellulose；
(2) the nanocrystalline starch of step (1) preparation, nano-cellulose are mixed with natural non-grain degradable starch, with uniformly
Dispersion, then carries out activation modification process；It is last again emulsion polymerization to be carried out to the dispersion after activation modification process, most
Eventually prepared nano-cellulose, nanocrystalline starch and non-grain degradable starch emulsion graft copolymer, i.e. nano-cellulose enhancement mode are given birth to
Thing base nano rubber latex.
2. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
The starch is one or more in corn starch, tapioca, potato starch, rice starch.
3. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
Plant fiber's cellulose fiber is one or more in lumber fibre, grass fiber, cotton fiber, flaxen fiber, pulp fibers.
4. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
Enzymolysis processing described in step (1), using compound cellulase, it contains endoglucanase (EG), exoglucanase
(CBH), cellobiose enzyme (BG)；Enzymolysis processing technique is：First, water is added in retort；Then, starch and fibre are weighed
Dimension raw material is added in retort, is made into the mixed liquor of 1～10% concentration, is stirred；Then, answering for 1.0～10.0FPU/g is added
Condensating fiber element enzyme, adds the pH value that buffer solution controls mixed liquor reaction system to be 5.0 ± 0.2, and controlling temperature of reaction system is
40～60 DEG C, the response time is 1～3h.Starch, the absolute dry mass ratio of Plant fiber's cellulose fiber are (1～30):1.
5. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
Chemical oxidation pre-treatment described in step (1), is added in the reaction system after starch, plant cellulose fiber enzymolysis processing
Chemical oxidation reagent, makes the starch after oxidation and the carboxyl-content of Plant fiber's cellulose fiber mixed liquor be at least up to 0.80mmol/g
And more than.
6. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 5, it is characterised in that：
The chemical oxidation reagent is 2,2,6,6- tetramethyl piperidine nitrogen oxides, sodium bromide, sodium metaperiodate, sodium hypochlorite, chlorous acid
Sodium or hydrogen peroxide.
7. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
Mechanical treatment described in step (1), is using high pressure homogenizer, grinding and crushing machine, sand mill, ball mill, supersonic cell powder
One or more in broken machine, to respectively through the starch and Plant fiber's cellulose fiber mixed liquor of enzymolysis and chemical oxidation treatment
Apply mechanism, obtain nanocrystalline starch and nano-cellulose with nano-scale；Wherein, the particle diameter of nanocrystalline starch is little
In 100nm, the fibril width of nano-cellulose is less than 100nm.
8. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
In step (2), starch and Plant fiber's cellulose fiber mixed liquor and the absolute dry mass ratio of natural non-grain degradable starch are (1～10):
100。
9. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, it is characterised in that：
Activation modification described in step (2) process be etherified, be esterified, be crosslinked in one or more of chemical modification process.
10. the preparation method of nano-cellulose enhancement mode bio-based nano rubber latex according to claim 1, its feature exists
In：Emulsion polymerization described in step (2) is to add initiator in the dispersion after activation modification process, causes double bond
The emulsion polymerization of class monomer.
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| CN109320617B (en) * | 2018-09-18 | 2021-01-29 | 青岛科技大学 | Bio-based nano material and preparation method thereof |
| CN112482083A (en) * | 2020-11-24 | 2021-03-12 | 中国制浆造纸研究院有限公司 | Starch-based compound capable of improving oil resistance of paper |
| CN115559147A (en) * | 2021-07-02 | 2023-01-03 | 中国制浆造纸研究院有限公司 | Method for improving nano-fibrillation efficiency of nano-cellulose |
| CN115559147B (en) * | 2021-07-02 | 2024-01-16 | 中国制浆造纸研究院有限公司 | Method for improving nano cellulose nano-fibrillation efficiency |
| CN114940843A (en) * | 2022-05-31 | 2022-08-26 | 深圳市凌普鑫科技有限公司 | High-stability water-based ink with surfactant and preparation method thereof |
| CN114805689A (en) * | 2022-06-01 | 2022-07-29 | 浙江歌瑞新材料有限公司 | Preparation method of nano-cellulose reinforced polyvinylidene fluoride composite material |
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