CN106676961A - Modified hogskin collagen sizing agent and preparation method thereof - Google Patents
Modified hogskin collagen sizing agent and preparation method thereof Download PDFInfo
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- CN106676961A CN106676961A CN201611127087.4A CN201611127087A CN106676961A CN 106676961 A CN106676961 A CN 106676961A CN 201611127087 A CN201611127087 A CN 201611127087A CN 106676961 A CN106676961 A CN 106676961A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
-
- 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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/18—Reinforcing agents
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
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Abstract
The invention provides a modified hogskin collagen sizing agent and a preparation method thereof. The preparation method comprises the following steps: taking fresh hogskin, cutting into pieces, removing fat, filtering, removing fat, filtering, cleaning with clear water twice, adding a sodium chloride solution, stirring, removing salt-soluble impure proteins, carrying out microwave radiation, adding a Tis-HCl buffer solution, trypsinase and papain to carry out extraction, inactivating the enzymes, centrifugating the extracting solution, carrying out freeze-drying on the supernate, adding deionized water, dissolving by heating and stirring, transferring the solution into a four-neck flask, heating, adding butyl acrylate and styrene, stirring, adding azodiisobutyronitrile to react, heating, adding danish agar, sodium caseinate and coco fatty acid diethanol amide, stirring, and naturally cooling. The invention aims to provide a modified hogskin collagen sizing agent; and the modified hogskin collagen sizing agent can effectively enhance the surface strength, tensile strength and ring crush compression resistance of paper, and has the advantages of low water-absorbing capacity and favorable water resistance.
Description
Technical field
The present invention relates to paper making additive field, and in particular to a kind of modified pigskin collagen sizing agent and its preparation side
Method.
Background technology
Whole world paper and paperboard production are huge, and among constantly developing, and for sustainable development, it is necessary to solve raw material
Shortage, energy shortage and it is seriously polluted the problems such as, while, it is necessary to develop the functional materials such as efficient sizing agent, reduce production cost,
Reduce environmental pollution, improve paper quality etc..Applying glue is the important upper skill of paper-making process, is to make paper table by certain process
Face forms a kind of lyophobicity film of mental retardation, so that paper and cardboard obtain the property for resisting fluid (referring mainly to water).Typically seek
Look for a kind of material with low surface free energy so as to be evenly distributed on paper surface, prevent or delays liquid is to paper fiber
Infiltration and diffusion, the material with this performance is referred to as glue used in paper-making.China is at present for the demand also right and wrong of paper
Chang Ju great, for the requirement also more and more higher of its performance, therefore, research and development can significantly improve the strength character of paper and anti-
The sizing agent of aqueouss energy is increased economic efficiency and is had great importance for paper industry technological progress.
The content of the invention
The technical problem to be solved：It is an object of the invention to provide a kind of modified pigskin collagen sizing agent, can be effective
Surface strength, tensile strength and the ring crush intensity of paper are improved, while water absorption is few, water repelling property is good.
Technical scheme：A kind of modified pigskin collagen sizing agent, is prepared from by following component：It is Corii Sus domestica 40-60g, red
Algin 2-4g, trypsin 0.1-0.15g, papain 0.05-0.1g, lauric acid amide of ethanol 2-4g, Sodium Chloride
0.5-0.8g, butyl acrylate 8-15g, sodium caseinate 1-2g, Tris-HCl buffer 40-50ml, sodium carbonate 4-5g, azo
Bis-isobutyronitrile 0.03-0.05g, styrene 15-25ml, chloroform 40-60ml, dehydrated alcohol 20-30ml, deionized water 230-
300ml。
It is further preferred that described a kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica
45-55g, Furcellaran 2.5-3.5g, trypsin 0.11-0.14g, papain 0.06-0.09g, coconut oil diethanol acyl
Amine 2.5-3.5g, Sodium Chloride 0.6-0.7g, butyl acrylate 10-13g, sodium caseinate 1.2-1.8g, Tris-HCl buffer
42-48ml, sodium carbonate 4-5g, azodiisobutyronitrile 0.04g, styrene 17-22ml, chloroform 45-55ml, dehydrated alcohol
22-28ml, deionized water 250-280ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is comprised the following steps：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 50-65ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 90-120ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Tis-HCl buffer, trypsin and wood are added after microwave exposure 1-5 minutes are carried out at temperature 20-30 DEG C
Melon protease carries out extracting 24-30 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Remaining deionized water is added, temperature is heated to for 40-50 DEG C, is stirred to dissolving, be transferred to reflux condensation mode
In pipe, motor stirrer, the four-hole boiling flask of nitrogen protection device, 70-80 DEG C is warming up to, adds butyl acrylate and styrene,
It is slowly stirred 30-40 minutes；
Step 6：Add azodiisobutyronitrile reaction 2-2.5 hours, be warming up to 80-90 DEG C, add Furcellaran, sodium caseinate and
Lauric acid amide of ethanol, stirs 0.5-1 hours under rotating speed 100-150r/min, naturally cools to room temperature and obtains final product.
It is further preferred that temperature is 25 DEG C in step 3, exposure time is 2-4 minutes, and extraction time is 25-28 hours.
It is further preferred that being heated to 45 DEG C in step 5 for the first time, 75 DEG C are warming up to for the second time, mixing time is 35 points
Clock.
It is further preferred that in step 6 response time be 2.25 hours, be warming up to 85 DEG C, rotating speed is 110-140r/min,
Mixing time is 0.75 hour.
Beneficial effect：The modified pigskin collagen sizing agent of the present invention can effectively improve the surface strength of paper, anti-tensile
Intensity and ring crush intensity, can reach respectively 1.72m/s, 2.68KN/m and 8.59Nm/g, the paper 30s water suctions of non-applying glue
Value reaches 116.2g/m2, and 30s hygroscopicity values are only 37.4g/m after paper sizing2, water absorption is few, and water repelling property is good.
Specific embodiment
Embodiment 1
A kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica 40g, Furcellaran 2g, trypsin
0.1g, papain 0.05g, lauric acid amide of ethanol 2g, Sodium Chloride 0.5g, butyl acrylate 8g, sodium caseinate 1g,
Tris-HCl buffer 40ml, sodium carbonate 4g, azodiisobutyronitrile 0.03g, styrene 15ml, chloroform 40ml, anhydrous second
Alcohol 20ml, deionized water 230ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 50ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 90ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Microwave exposure is carried out at 20 DEG C of temperature Tis-HCl buffer, trypsin and Fructus Chaenomeliss egg are added after 1 minute
White enzyme carries out extracting 24 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Add remaining deionized water, be heated to temperature for 40 DEG C, stir to dissolving, be transferred to reflux condensing tube,
In motor stirrer, the four-hole boiling flask of nitrogen protection device, 70 DEG C are warming up to, add butyl acrylate and styrene, slowly stirred
Mix 30 minutes；
Step 6：Add azodiisobutyronitrile to react 2 hours, be warming up to 80 DEG C, add Furcellaran, sodium caseinate and coconut oil
Diglycollic amide, stirs 0.5 hour under rotating speed 100r/min, naturally cools to room temperature and obtains final product.
Embodiment 2
A kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica 45g, Furcellaran 2.5g, trypsin
0.11g, papain 0.06g, lauric acid amide of ethanol 2.5g, Sodium Chloride 0.6g, butyl acrylate 10g, caseinic acid
Sodium 1.2g, Tris-HCl buffer 42ml, sodium carbonate 4g, azodiisobutyronitrile 0.04g, styrene 17ml, chloroform 45ml,
Dehydrated alcohol 22ml, deionized water 250ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 55ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 100ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Microwave exposure is carried out at 25 DEG C of temperature Tis-HCl buffer, trypsin and Fructus Chaenomeliss egg are added after 2 minutes
White enzyme carries out extracting 25 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Add remaining deionized water, be heated to temperature for 45 DEG C, stir to dissolving, be transferred to reflux condensing tube,
In motor stirrer, the four-hole boiling flask of nitrogen protection device, 75 DEG C are warming up to, add butyl acrylate and styrene, slowly stirred
Mix 35 minutes；
Step 6：Add azodiisobutyronitrile to react 2.25 hours, be warming up to 85 DEG C, add Furcellaran, sodium caseinate and cocos nucifera oil
Sour diglycollic amide, stirs 0.75 hour under rotating speed 110r/min, naturally cools to room temperature and obtains final product.
Embodiment 3
A kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica 50g, Furcellaran 3g, trypsin
0.12g, papain 0.075g, lauric acid amide of ethanol 3g, Sodium Chloride 0.65g, butyl acrylate 11.5g, casein
Sour sodium 1.5g, Tris-HCl buffer 45ml, sodium carbonate 4.5g, azodiisobutyronitrile 0.04g, styrene 20ml, chloroform
50ml, dehydrated alcohol 25ml, deionized water 265ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 57ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 105ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Microwave exposure is carried out at 25 DEG C of temperature Tis-HCl buffer, trypsin and Fructus Chaenomeliss egg are added after 3 minutes
White enzyme carries out extracting 27 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Add remaining deionized water, be heated to temperature for 45 DEG C, stir to dissolving, be transferred to reflux condensing tube,
In motor stirrer, the four-hole boiling flask of nitrogen protection device, 75 DEG C are warming up to, add butyl acrylate and styrene, slowly stirred
Mix 35 minutes；
Step 6：Add azodiisobutyronitrile to react 2.25 hours, be warming up to 85 DEG C, add Furcellaran, sodium caseinate and cocos nucifera oil
Sour diglycollic amide, stirs 0.75 hour under rotating speed 125r/min, naturally cools to room temperature and obtains final product.
Embodiment 4
A kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica 55g, Furcellaran 3.5g, trypsin
0.14g, papain 0.09g, lauric acid amide of ethanol 3.5g, Sodium Chloride 0.7g, butyl acrylate 13g, caseinic acid
Sodium 1.8g, Tris-HCl buffer 48ml, sodium carbonate 5g, azodiisobutyronitrile 0.04g, styrene 22ml, chloroform 55ml,
Dehydrated alcohol 28ml, deionized water 280ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 60ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 110ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Microwave exposure is carried out at 25 DEG C of temperature Tis-HCl buffer, trypsin and Fructus Chaenomeliss egg are added after 4 minutes
White enzyme carries out extracting 28 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Add remaining deionized water, be heated to temperature for 45 DEG C, stir to dissolving, be transferred to reflux condensing tube,
In motor stirrer, the four-hole boiling flask of nitrogen protection device, 75 DEG C are warming up to, add butyl acrylate and styrene, slowly stirred
Mix 35 minutes；
Step 6：Add azodiisobutyronitrile to react 2.25 hours, be warming up to 85 DEG C, add Furcellaran, sodium caseinate and cocos nucifera oil
Sour diglycollic amide, stirs 0.75 hour under rotating speed 140r/min, naturally cools to room temperature and obtains final product.
Embodiment 5
A kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica 60g, Furcellaran 4g, trypsin
0.15g, papain 0.1g, lauric acid amide of ethanol 4g, Sodium Chloride 0.8g, butyl acrylate 15g, sodium caseinate
It is 2g, Tris-HCl buffer 50ml, sodium carbonate 5g, azodiisobutyronitrile 0.05g, styrene 25ml, chloroform 60ml, anhydrous
Ethanol 30ml, deionized water 300ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 65ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 120ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Microwave exposure is carried out at 30 DEG C of temperature Tis-HCl buffer, trypsin and Fructus Chaenomeliss egg are added after 5 minutes
White enzyme carries out extracting 30 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Add remaining deionized water, be heated to temperature for 50 DEG C, stir to dissolving, be transferred to reflux condensing tube,
In motor stirrer, the four-hole boiling flask of nitrogen protection device, 80 DEG C are warming up to, add butyl acrylate and styrene, slowly stirred
Mix 40 minutes；
Step 6：Add azodiisobutyronitrile to react 2.5 hours, be warming up to 90 DEG C, add Furcellaran, sodium caseinate and cocos nucifera oil
Sour diglycollic amide, stirs 1 hour under rotating speed 150r/min, naturally cools to room temperature and obtains final product.
Comparative example 1
The present embodiment is not contain butyl acrylate, styrene and azodiisobutyronitrile with the difference of embodiment 1.Specifically
It is：
A kind of modified pigskin collagen sizing agent, is prepared from by following component：Corii Sus domestica 40g, Furcellaran 2g, trypsin
0.1g, papain 0.05g, lauric acid amide of ethanol 2g, Sodium Chloride 0.5g, sodium caseinate 1g, Tris-HCl buffering
Liquid 40ml, sodium carbonate 4g, chloroform 40ml, dehydrated alcohol 20ml, deionized water 230ml.
The preparation method of above-mentioned modified pigskin collagen sizing agent is：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 50ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 90ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Microwave exposure is carried out at 20 DEG C of temperature Tis-HCl buffer, trypsin and Fructus Chaenomeliss egg are added after 1 minute
White enzyme carries out extracting 24 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Add remaining deionized water, be heated to temperature for 40 DEG C, stir to dissolving, be warming up to 80 DEG C, add Furcellaran,
Sodium caseinate and lauric acid amide of ethanol, stir 0.5 hour under rotating speed 100r/min, naturally cool to room temperature and obtain final product.
1 is see the table below with the performance of paper after sizing agent of the present invention, resin added is 50g/m2, it may be seen that addition
The surface strength of paper, tensile strength and ring crush intensity are all significantly improved after sizing agent, and 1.72m/ is can reach respectively
S, 2.68KN/m and 8.59Nm/g, the paper 30s hygroscopicity values of non-applying glue reach 116.2g/m2, and 30s water suctions after paper sizing
Value is only 37.4g/m2, water absorption is few, and water repelling property is good.
The partial properties index of paper after the modified pigskin collagen sizing agent of the addition of table 1
| Name of product | Surface strength（m/s） | Tensile index（KN/m） | Ring crush index（N·m/g) | 30s hygroscopicity values（g/m2） |
| Embodiment 1 | 1.61 | 2.56 | 8.43 | 39.1 |
| Embodiment 2 | 1.64 | 2.61 | 8.51 | 38.6 |
| Embodiment 3 | 1.68 | 2.64 | 8.55 | 38.2 |
| Embodiment 4 | 1.72 | 2.68 | 8.59 | 37.4 |
| Embodiment 5 | 1.71 | 2.66 | 8.57 | 37.8 |
| Comparative example 1 | 1.52 | 2.41 | 7.61 | 50.2 |
| Non- applying glue | 1.15 | 1.21 | 2.83 | 116.2 |
Claims (6)
1. a kind of modified pigskin collagen sizing agent, it is characterised in that：It is prepared from by following component：It is Corii Sus domestica 40-60g, red
Algin 2-4g, trypsin 0.1-0.15g, papain 0.05-0.1g, lauric acid amide of ethanol 2-4g, Sodium Chloride
0.5-0.8g, butyl acrylate 8-15g, sodium caseinate 1-2g, Tris-HCl buffer 40-50ml, sodium carbonate 4-5g, azo
Bis-isobutyronitrile 0.03-0.05g, styrene 15-25ml, chloroform 40-60ml, dehydrated alcohol 20-30ml, deionized water 230-
300ml。
2. a kind of modified pigskin collagen sizing agent according to claim 1, it is characterised in that：Prepared by following component
Form：Corii Sus domestica 45-55g, Furcellaran 2.5-3.5g, trypsin 0.11-0.14g, papain 0.06-0.09g, coconut oil
Diglycollic amide 2.5-3.5g, Sodium Chloride 0.6-0.7g, butyl acrylate 10-13g, sodium caseinate 1.2-1.8g, Tris-
HCl buffer 42-48ml, sodium carbonate 4-5g, azodiisobutyronitrile 0.04g, styrene 17-22ml, chloroform 45-55ml,
Dehydrated alcohol 22-28ml, deionized water 250-280ml.
3. the preparation method of a kind of modified pigskin collagen sizing agent described in any one of claim 1 to 2, its feature exists
In：Comprise the following steps：
Step 1：The fritter that fresh porcine skin is cut into 10mm × 10mm is taken, adds chloroform and dehydrated alcohol to carry out the de- of fat
Remove, filter, the solution for adding sodium carbonate and 50-65ml deionized waters removes again fat, clean water 2 times is gone after filtration；
Step 2：Sodium Chloride and 90-120ml deionized water solutions, stirring is added to remove desalination dissolubility foreign protein；
Step 3：Tis-HCl buffer, trypsin and wood are added after microwave exposure 1-5 minutes are carried out at temperature 20-30 DEG C
Melon protease carries out extracting 24-30 hours；
Step 4：After enzyme denaturing, extracting solution is centrifuged, then supernatant is carried out into lyophilization；
Step 5：Remaining deionized water is added, temperature is heated to for 40-50 DEG C, is stirred to dissolving, be transferred to reflux condensation mode
In pipe, motor stirrer, the four-hole boiling flask of nitrogen protection device, 70-80 DEG C is warming up to, adds butyl acrylate and styrene,
It is slowly stirred 30-40 minutes；
Step 6：Add azodiisobutyronitrile reaction 2-2.5 hours, be warming up to 80-90 DEG C, add Furcellaran, sodium caseinate and
Lauric acid amide of ethanol, stirs 0.5-1 hours under rotating speed 100-150r/min, naturally cools to room temperature and obtains final product.
4. the preparation method of a kind of modified pigskin collagen sizing agent according to claim 3, it is characterised in that：It is described
Temperature is 25 DEG C in step 3, and exposure time is 2-4 minutes, and extraction time is 25-28 hours.
5. the preparation method of a kind of modified pigskin collagen sizing agent according to claim 3, it is characterised in that：It is described
It is heated to 45 DEG C in step 5 for the first time, 75 DEG C is warming up to for the second time, mixing time is 35 minutes.
6. the preparation method of a kind of modified pigskin collagen sizing agent according to claim 3, it is characterised in that：It is described
The response time is 2.25 hours in step 6, is warming up to 85 DEG C, and rotating speed is 110-140r/min, and mixing time is 0.75 hour.
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| CN108411632A (en) * | 2018-04-10 | 2018-08-17 | 佛山市熙华科技有限公司 | A kind of preparation method of environment-friendly type cotton finishing agent |
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| CN101649583A (en) * | 2009-09-01 | 2010-02-17 | 东莞市清正合成高新材料有限公司 | Cation surface sizing agent and preparation method thereof |
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Application publication date: 20170517 |
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