CN107603535A - A kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity - Google Patents
A kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity Download PDFInfo
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- CN107603535A CN107603535A CN201710933679.3A CN201710933679A CN107603535A CN 107603535 A CN107603535 A CN 107603535A CN 201710933679 A CN201710933679 A CN 201710933679A CN 107603535 A CN107603535 A CN 107603535A
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Abstract
The present invention relates to technical field of adhesive preparation, and in particular to a kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity.The present invention has the advantages that volatility is good and harmless to human body, can make the toxicity of adhesive reduce to discard in tealeaves obtained concentrate as solvent.White clouds building stones are rich in magnesium salts and calcium salt, chloroprene rubber adhesive agent is after the nucleus generation of low temperature, growth course can be influenceed and be suppressed by the three-dimensional effect that metal salt crystallizes, the cross-linked network formed after neoprene grafted propylene acid declines the shrinkage of neoprene, it is unfavorable for the regularly arranged formation nucleus of neoprene, avoids neoprene low temperature from easily crystallizing the purpose hardened so as to reach.
Description
Technical field
The present invention relates to technical field of adhesive preparation, and in particular to a kind of preparation side of the cold-resistant chloroprene rubber adhesive agent of low toxicity
Method.
Background technology
Rubber adhesive all occupies very important in the numerous areas of national economy and the various aspects of daily life
Status, wherein, neoprene adhesive（Abbreviation chloroprene rubber adhesive agent）It is Typical Representative.Chloroprene rubber adhesive agent is a kind of solvent-borne type rubber
Adhesive.The chloroprene rubber adhesive agent method routinely prepared, main component are highly crystalline type neoprene, tackifier, solvent, auxiliary agent
Deng, there are raw material ample supply and prompt delivery and cost is low, production is simple, and the initial bonding strength of adhesive is big, and adhesive strength is high, good weatherability,
The features such as applied widely.It is widely used in the industries such as furniture, leather, building, interior decoration.
The organic solvent that traditional chloroprene rubber adhesive agent uses is mostly the high toxicity solvents such as benzene, dimethylbenzene, toluene, although national
It is made that regulation limits to this, but not total ban, most businessmans still use a large amount of toluene, to environment and constructor
Body brings very big injury.Although the neoprene for having some businessmans to have developed some low toxic and environment-friendly types, nearly all contains
Ethyl acetate, acetone, butanone etc. have the solvent of intense irritation smell, so that bringing very big inconvenience for construction.Meanwhile
The chelate that the tackifier used in chloroprene rubber adhesive agent are usually tert butyl phenolic resin and magnesia is prepared, is existed in phenolic resin
The release of a certain amount of free formaldehyde, particularly free formaldehyde is a slow process, and these unfavorable factor long lasting effects
Environmental and human health impacts.Therefore, national Minister of the General Administration for Quality Supervision has issued national standard《GB18583-2008 indoor decorating and refurnishing materials are gluing
Limits of harmful substances in agent》, toxicity and the harm therein for providing to greatly reduce chloroprene rubber adhesive agent.From environmental protection and human body
For the angle of health, one cuts with Form aldehyde release and the adhesive containing toxic larger solvent, all should progressively withdraw from the market,
And substituted by no Form aldehyde release, the less product of toxicity be the development of following adhesive main trend.It is however, molten from low toxicity
Agent system, then need the factors such as integrated survey its dissolubility, evaporation rate, reactivity.Other chloroprene rubber adhesive agent cold resistance is poor, is adding
Man-hour is sensitive to technological temperature, and difficulty is brought to operation, requires high to storage environment.
From above-mentioned a variety of application requirements, the good chloroprene rubber adhesive agent of a kind of low toxic and environment-friendly, cold resistance is developed with very big
Practicality and necessity.
The content of the invention
Present invention mainly solves technical problem, for chloroprene rubber adhesive agent strong toxicity, low temperature easily crystallization harden the defects of, carry
A kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity is supplied.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity, it is characterised in that specifically preparation process is：
（1）100~110g chlorobutadienes are added in the three-necked flask with agitator and thermometer, added into three-necked flask
Sodium hydroxide solution that 100~120mL mass fractions are 5%, 30~40mL mass fractions are 8% sodium carbonate liquor, 50~60mL
Mass fraction is 28% mahogany acid sodium solution, 100~110mL deionized waters, starts agitator, is stirred with 80~90r/min rotating speeds
After mixing 10~15min of emulsification, 1~3g potassium peroxydisulfates are added, 45~48 DEG C is heated to, 3~4h of insulation reaction, obtains neoprene
Latex；
（2）Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, former roll temperature is 45~50 DEG C, and rear roll temperature is 35~45
DEG C, roll spacing starts refining glue under conditions of being 7~9mm, and after plasticating 2~3 times, 10~15gMgO, 20 are sequentially added into rubber mixing machine
After~30g White Carbon blacks and 5~7g beta-naphthylamines, continue to plasticate condition mixing refining glue by original, neoprene is obtained, with bale splitter by chlorine
Buna is shredded, and obtains neoprene sheet；
（3）80~90g tealeaves discarded is put into cloth bag, it is 20% sodium carbonate that cloth bag is put into 150~180mL mass fractions
In solution, 3~4h is soaked, liquid in cloth bag is extracted, obtains soak, by soak
It is placed in beaker, adds 40~50mL absolute ethyl alcohols, be heated to 90~100 DEG C, 0.5~1.0h of insulated and stirred, obtain
To concentrate；
（4）Weigh 800~900g dolomites and 2~3h is ground in stone mill, grinding crosses 100 mesh standard sieves after terminating and obtains white clouds
Stone powder, dolomite powder is put into calcining furnace, is heated to 800~900 DEG C, insulation 3~5h of calcining, is cooled to room temperature
After discharge, obtain light dolomite material；
（5）Count in parts by weight, 20~30 portions of concentrates of addition into the 100mL four-hole bottles with stirring and reflux, 30
~40 parts of light dolomite material, 80~90 parts of neoprene sheets are added, are heated to 65~70 DEG C,
Start agitator, 30~40min is stirred with 200~250r/min rotating speed, after neoprene sheet dissolving, to three-necked flask
Middle addition 1~3g potassium peroxydisulfates, after continuing 15~20min of stirring, 40~50 parts of acrylic acid are added, continue heat temperature raising 80~85
DEG C, 30~45min is reacted, 10~20 parts of benzoyl peroxides is added, is cooled to 40~45 DEG C, it is resistance to obtain sticky glue i.e. low toxicity
Cold chloroprene rubber adhesive agent.
A kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity, it is characterised in that specifically preparation process is：
（1）100~110g chlorobutadienes are added in the three-necked flask with agitator and thermometer, added into three-necked flask
100~120mL sodium hydroxide solutions, 30~40mL sodium carbonate liquors, 50~60mL mahogany acids sodium solution, 100~110mL are gone
Ionized water, start agitator, after stirring and emulsifying, add 1~3g potassium peroxydisulfates, heat temperature raising, insulation reaction, obtain neoprene
Breast；
（2）Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, sequentially added in backward rubber mixing machine of plasticating 10~15gMgO, 20~
After 30g White Carbon blacks and 5~7g beta-naphthylamines, continue to plasticate condition mixing refining glue by original, neoprene is obtained, with bale splitter by neoprene
Rubber shreds, and obtains neoprene sheet；
（3）80~90g tealeaves discarded is put into cloth bag, cloth bag is put into 150~180mL sodium carbonate liquors, is soaked, will
Liquid is extracted in cloth bag, obtains soak, and soak is placed in beaker, is added 40~50mL absolute ethyl alcohols, heat temperature raising, is protected
Temperature stirring, obtains concentrate；
（4）Weigh 800~900g dolomites to grind in stone mill, grinding crosses standard screen after terminating and obtains dolomite powder, will
Dolomite powder is put into calcining furnace, heat temperature raising, insulation calcining, is discharged after being cooled to room temperature, is obtained light dolomite material；
（5）Count in parts by weight, 20~30 portions of concentrates of addition into the four-hole bottle with stirring and reflux, 30~40 parts
Light dolomite material, 80~90 parts of neoprene sheets are added, heat temperature raising, start agitator, are stirred, after neoprene sheet dissolving,
1~3g potassium peroxydisulfates are added into three-necked flask, after continuing stirring, 40~50 parts of acrylic acid is added, continues heat temperature raising, instead
Should, 10~20 parts of benzoyl peroxides are added, cooling, obtain sticky glue i.e..
Step（1）Described sodium hydroxide solution, sodium carbonate liquor, the mass fraction of mahogany acid sodium solution are respectively 5%
, 8%, 28%, speed of agitator is 80~90r/min, and the stirring and emulsifying time is 10~15min, and temperature is 45~48 after heat temperature raising
DEG C, the insulation reaction time is 3~4h.
Step（2）The described condition of plasticating in rubber mixing machine is：Preceding roll temperature is 45~50 DEG C, and rear roll temperature is 35~45
DEG C, roll spacing is 7~9mm.
Step（3）Described mass fraction is 20%, and soak time be 3~4h, and temperature is 90~100 DEG C after heat temperature raising,
The insulated and stirred time is 0.5~1.0h.
Step（4）Described milling time is 2~3h, and the specification of sieve is 100 mesh, and temperature is 800~900 after heat temperature raising
DEG C, insulation calcination time is 3~5h.
Step（5）Temperature is 65~70 DEG C after described heat temperature raising, and speed of agitator is 200~250r/min, during stirring
Between be 30~40min, continuation mixing time is 15~20min, and the reaction time is 30~45min, after cooling temperature be 40~45
℃。
The beneficial effects of the invention are as follows：
（1）It is dense to be obtained in discarded tealeaves without volatile solvents such as ethyl acetate, ketone and formaldehyde in solvent in the present invention
Contracting liquid contains catechin as solvent in concentrate, and catechin belongs to flavanols, and volatility is good but harmless to human body, and
Contain a small amount of Tea Polyphenols in concentrate, there is anticancer function, so that the toxicity of adhesive reduces；
（2）Light dolomite material is rich in magnesium salts and calcium salt in the present invention, and chloroprene rubber adhesive agent grew after the nucleus generation of low temperature
Journey can be influenceed by the three-dimensional effect that metal salt crystallizes and be suppressed, the cross-linked network formed after neoprene grafted propylene acid
Decline the shrinkage of neoprene, be unfavorable for the regularly arranged formation nucleus of neoprene, neoprene rubber is avoided so as to reach
Glue low temperature easily crystallizes the purpose hardened.
Embodiment
100~110g chlorobutadienes are added in the three-necked flask with agitator and thermometer, 100 are added into three-necked flask
Sodium hydroxide solution that~120mL mass fractions are 5%, 30~40mL mass fractions are 8% sodium carbonate liquor, 50~60mL mass
Fraction is 28% mahogany acid sodium solution, 100~110mL deionized waters, starts agitator, and breast is stirred with 80~90r/min rotating speeds
After changing 10~15min, 1~3g potassium peroxydisulfates are added, 45~48 DEG C is heated to, 3~4h of insulation reaction, obtains neoprene
Breast；Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, former roll temperature is 45~50 DEG C, and rear roll temperature is 35~45 DEG C, roller
Away from refining glue is started for 7~9mm condition, after plasticating 2~3 times, it is white that 10~15gMgO, 20~30g are sequentially added into rubber mixing machine
After carbon black and 5~7g beta-naphthylamines, continue to plasticate condition mixing refining glue by original, neoprene is obtained, with bale splitter by neoprene
Chopping, obtains neoprene sheet；80~90g tealeaves discarded is put into cloth bag, cloth bag is put into 150~180mL mass fractions
In 20% sodium carbonate liquor, to soak 3~4h, liquid in cloth bag being extracted, obtains soak, soak is placed in beaker, is added
Enter 40~50mL absolute ethyl alcohols, be heated to 90~100 DEG C, 0.5~1.0h of insulated and stirred, obtain concentrate；Weigh 800~
900g dolomites grind 2~3h in stone mill, and grinding crosses 100 mesh standard sieves after terminating and obtains dolomite powder, by dolomite
Powder is put into calcining furnace, is heated to 800~900 DEG C, insulation 3~5h of calcining, is discharged, obtain light-burned after being cooled to room temperature
White clouds building stones；Count in parts by weight, 20~30 portions of concentrates of addition into the four-hole bottle with stirring and reflux, 30~40
Part light dolomite material, 80~90 parts of neoprene sheets are added, be heated to 65~70 DEG C, start agitator, with 200~
250r/min rotating speed stirs 30~40min, and after neoprene sheet dissolving, 1~3g potassium peroxydisulfates are added into three-necked flask, after
After 15~20min of continuous stirring, 40~50 parts of acrylic acid are added, continues to be heated to 80~85 DEG C, reacts 30~45min, add
Enter 10~20 parts of benzoyl peroxides, be cooled to 40~45 DEG C, discharging, obtain the cold-resistant chloroprene rubber adhesive agent of sticky glue i.e. low toxicity.
Example 1
100g chlorobutadienes are added in the three-necked flask with agitator and thermometer, 100mL matter is added into three-necked flask
Measure fraction be 5% sodium hydroxide solution, 30mL mass fractions be 8% sodium carbonate liquor, 50mL mass fractions be 28% mahogany acid
Sodium solution, 100mL deionized waters, start agitator, after 80r/min rotating speed stirring and emulsifyings 10min, add 1g potassium peroxydisulfates,
45 DEG C are heated to, insulation reaction 3h, obtains polychloroprene latex；Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, with preliminary roller
Temperature is 45 DEG C, and rear roll temperature is 35 DEG C, and roll spacing is that 7mm condition starts refining glue, after plasticating 2 times, is added successively into rubber mixing machine
After entering 10gMgO, 20g White Carbon black and 5g beta-naphthylamines, continue by original plasticate condition mixing refining glue, obtain neoprene, use bale splitter
Neoprene is shredded, obtains neoprene sheet；The 80g tealeaves discarded is put into cloth bag, cloth bag is put into 150mL mass fractions
In 20% sodium carbonate liquor, to soak 3h, liquid in cloth bag being extracted, obtains soak, soak is placed in beaker, add
40mL absolute ethyl alcohols, 90 DEG C are heated to, insulated and stirred 0.5h, obtains concentrate；800g dolomites are weighed in stone mill
2h is ground, grinding crosses 100 mesh standard sieves after terminating and obtains dolomite powder, dolomite powder is put into calcining furnace, and heating rises
Temperature insulation calcining 3h, discharges after being cooled to room temperature to 800 DEG C, obtains light dolomite material；Count in parts by weight, to stirring
Mix and the four-hole bottle of reflux in add 20 portions of concentrates, 30 parts of light dolomite material, add 80 parts of neoprene sheets, heating rise
Temperature starts agitator to 65 DEG C, and 30min is stirred with 200r/min rotating speed, after neoprene sheet dissolving, adds into three-necked flask
Enter 1g potassium peroxydisulfates, continue after stirring 15min, add 40 parts of acrylic acid, continue to be heated to 80 DEG C, react 30min, add
10 parts of benzoyl peroxides, 40 DEG C are cooled to, discharging, obtains the cold-resistant chloroprene rubber adhesive agent of sticky glue i.e. low toxicity.
Example 2
110g chlorobutadienes are added in the three-necked flask with agitator and thermometer, 120mL matter is added into three-necked flask
Measure fraction be 5% sodium hydroxide solution, 40mL mass fractions be 8% sodium carbonate liquor, 60mL mass fractions be 28% mahogany acid
Sodium solution, 110mL deionized waters, start agitator, after 90r/min rotating speed stirring and emulsifyings 15min, add 3g potassium peroxydisulfates,
48 DEG C are heated to, insulation reaction 4h, obtains polychloroprene latex；Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, with preliminary roller
Temperature is 50 DEG C, and rear roll temperature is 45 DEG C, and roll spacing is that 9mm condition starts refining glue, after plasticating 3 times, is added successively into rubber mixing machine
After entering 15gMgO, 30g White Carbon black and 7g beta-naphthylamines, continue by original plasticate condition mixing refining glue, obtain neoprene, use bale splitter
Neoprene is shredded, obtains neoprene sheet；The 90g tealeaves discarded is put into cloth bag, cloth bag is put into 180mL mass fractions
In 20% sodium carbonate liquor, to soak 4h, liquid in cloth bag being extracted, obtains soak, soak is placed in beaker, add
50mL absolute ethyl alcohols, 100 DEG C are heated to, insulated and stirred 1.0h, obtains concentrate；900g dolomites are weighed in stone mill
3h is ground, grinding crosses 100 mesh standard sieves after terminating and obtains dolomite powder, dolomite powder is put into calcining furnace, and heating rises
Temperature insulation calcining 5h, discharges after being cooled to room temperature to 900 DEG C, obtains light dolomite material；Count in parts by weight, to stirring
Mix and the four-hole bottle of reflux in add 30 portions of concentrates, 40 parts of light dolomite material, add 90 parts of neoprene sheets, heating
70 DEG C are warming up to, starts agitator, 40min is stirred with 250r/min rotating speed, after neoprene sheet dissolving, into three-necked flask
3g potassium peroxydisulfates are added, continues after stirring 20min, adds 50 parts of acrylic acid, continues to be heated to 85 DEG C, reacts 45min, add
Enter 20 parts of benzoyl peroxides, be cooled to 45 DEG C, discharging, obtain the cold-resistant chloroprene rubber adhesive agent of sticky glue i.e. low toxicity.
Example 3
105g chlorobutadienes are added in the three-necked flask with agitator and thermometer, 110mL matter is added into three-necked flask
Measure fraction be 5% sodium hydroxide solution, 35mL mass fractions be 8% sodium carbonate liquor, 55mL mass fractions be 28% mahogany acid
Sodium solution, 105mL deionized waters, start agitator, after 85r/min rotating speed stirring and emulsifyings 13min, add 2g potassium peroxydisulfates,
46 DEG C are heated to, insulation reaction 3.5h, obtains polychloroprene latex；Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, in the past
Roll temperature is 47 DEG C, and rear roll temperature is 40 DEG C, and roll spacing is that 8mm condition starts refining glue, after plasticating 2 times, into rubber mixing machine successively
After adding 13gMgO, 25g White Carbon black and 6g beta-naphthylamines, continue to plasticate condition mixing refining glue by original, obtain neoprene, with cutting glue
Machine shreds neoprene, obtains neoprene sheet；The 85g tealeaves discarded is put into cloth bag, cloth bag is put into 160mL mass point
Number is in 20% sodium carbonate liquor, soaks 3.5h, liquid in cloth bag is extracted, obtains soak, soak is placed in beaker,
45mL absolute ethyl alcohols are added, 95 DEG C is heated to, insulated and stirred 0.8h, obtains concentrate；850g dolomites are weighed in grinding stone
2.5h is ground in machine, grinding crosses 100 mesh standard sieves after terminating and obtains dolomite powder, dolomite powder is put into calcining furnace,
850 DEG C are heated to, insulation calcining 4h, is discharged after being cooled to room temperature, obtains light dolomite material；Count in parts by weight, to
25 portions of concentrates are added in four-hole bottle with stirring and reflux, 35 parts of light dolomite material, add 85 parts of neoprene sheets,
67 DEG C are heated to, starts agitator, 35min is stirred with 230r/min rotating speed, after neoprene sheet dissolving, is burnt to three mouthfuls
2g potassium peroxydisulfates are added in bottle, continues after stirring 18min, adds 45 parts of acrylic acid, continue to be heated to 82 DEG C, reaction
37min, 15 parts of benzoyl peroxides are added, be cooled to 43 DEG C, discharging, obtain the cold-resistant chloroprene rubber adhesive agent of sticky glue i.e. low toxicity.
Comparative example
With the chloroprene rubber adhesive agent of company of Beijing production as a comparison case to chloroprene rubber adhesive agent produced by the present invention and comparative example
In chloroprene rubber adhesive agent detected, testing result is as shown in table 1：1st, method of testing
Viscosity test is detected by the measure of GB/T2794-2013 adhesive viscosity.
Content of formaldehyde determines the regulation by limits of harmful substances in GB/18583-2008 indoor decorating and refurnishing materials adhesives
Detected.
Non-volatile content measure is detected by the regulation of GB/T2793 adhesive non-volatile contents.
Bin stability is measured according to GB/T14074-2006 based Wood Adhesives and its resin method of inspection.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Viscosity（mPa·s） | 4120 | 4152 | 4173 | 3350 |
| Non-volatile content（%） | 32.5 | 33.2 | 34.1 | 28.0 |
| Free formaldehyde content（g·kg-1） | Do not detect | Do not detect | Do not detect | 0.743 |
| Bin stability（- 7 DEG C 30 days） | It is not stratified | It is not stratified | It is not stratified | Layering |
It can be seen from data in table 1, chloroprene rubber adhesive agent viscosity produced by the present invention is strong, low temperature resistant effect is good and low toxic and environment-friendly, tool
There is wide prospect of the application.
Claims (6)
1. a kind of preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity, it is characterised in that specifically preparation process is：
（1）100~110g chlorobutadienes are added in the three-necked flask with agitator and thermometer, added into three-necked flask
100~120mL sodium hydroxide solutions, 30~40mL sodium carbonate liquors, 50~60mL mahogany acids sodium solution, 100~110mL are gone
Ionized water, start agitator, after stirring and emulsifying, add 1~3g potassium peroxydisulfates, heat temperature raising, insulation reaction, obtain neoprene
Breast；
（2）Above-mentioned polychloroprene latex is put into rubber mixing machine and plasticated, sequentially added in backward rubber mixing machine of plasticating 10~15gMgO, 20~
After 30g White Carbon blacks and 5~7g beta-naphthylamines, continue to plasticate condition mixing refining glue by original, neoprene is obtained, with bale splitter by neoprene
Rubber shreds, and obtains neoprene sheet；
（3）80~90g tealeaves discarded is put into cloth bag, cloth bag is put into 150~180mL sodium carbonate liquors, is soaked, will
Liquid is extracted in cloth bag, obtains soak, and soak is placed in beaker, is added 40~50mL absolute ethyl alcohols, heat temperature raising, is protected
Temperature stirring, obtains concentrate；
（4）Weigh 800~900g dolomites to grind in stone mill, grinding crosses standard screen after terminating and obtains dolomite powder, will
Dolomite powder is put into calcining furnace, heat temperature raising, insulation calcining, is discharged after being cooled to room temperature, is obtained light dolomite material；
（5）Count in parts by weight, 20~30 portions of concentrates of addition into the four-hole bottle with stirring and reflux, 30~40 parts
Light dolomite material, 80~90 parts of neoprene sheets are added, heat temperature raising, start agitator, are stirred, after neoprene sheet dissolving,
1~3g potassium peroxydisulfates are added into three-necked flask, after continuing stirring, 40~50 parts of acrylic acid is added, continues heat temperature raising, instead
Should, 10~20 parts of benzoyl peroxides are added, cooling, obtain sticky glue i.e..
A kind of 2. preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity according to claim 1, it is characterised in that：Step（1）
Described sodium hydroxide solution, sodium carbonate liquor, the mass fraction of mahogany acid sodium solution are respectively 5%, 8%, 28%, stirring
Rotating speed is 80~90r/min, and the stirring and emulsifying time is 10~15min, and temperature is 45~48 DEG C after heat temperature raising, during insulation reaction
Between be 3~4h.
A kind of 3. preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity according to claim 1, it is characterised in that：Step（2）
The described condition of plasticating in rubber mixing machine is：Preceding roll temperature be 45~50 DEG C, rear roll temperature be 35~45 DEG C, roll spacing be 7~
9mm。
A kind of 4. preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity according to claim 1, it is characterised in that：Step（3）
Described mass fraction is 20%, and soak time be 3~4h, and temperature is 90~100 DEG C after heat temperature raising, and the insulated and stirred time is
0.5~1.0h.
A kind of 5. preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity according to claim 1, it is characterised in that：Step（4）
Described milling time is 2~3h, and the specification of sieve is 100 mesh, and temperature is 800~900 DEG C after heat temperature raising, is incubated calcination time
For 3~5h.
A kind of 6. preparation method of the cold-resistant chloroprene rubber adhesive agent of low toxicity according to claim 1, it is characterised in that：Step（5）
Temperature is 65~70 DEG C after described heat temperature raising, and speed of agitator is 200~250r/min, and mixing time is 30~40min, after
Continuous mixing time is 15~20min, and the reaction time is 30~45min, and temperature is 40~45 DEG C after cooling.
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| CN109762622A (en) * | 2019-02-25 | 2019-05-17 | 谭祖伍 | A kind of preparation method of oxidizing solids |
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| CN109536088A (en) * | 2018-10-29 | 2019-03-29 | 许水仙 | A kind of preparation method of lower shrinkage Heraeus |
| CN109762622A (en) * | 2019-02-25 | 2019-05-17 | 谭祖伍 | A kind of preparation method of oxidizing solids |
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