CN108624269A - A kind of rubber adhesive and preparation method thereof - Google Patents
A kind of rubber adhesive and preparation method thereof Download PDFInfo
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- CN108624269A CN108624269A CN201810359669.8A CN201810359669A CN108624269A CN 108624269 A CN108624269 A CN 108624269A CN 201810359669 A CN201810359669 A CN 201810359669A CN 108624269 A CN108624269 A CN 108624269A
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- adhesive
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- reaction kettle
- stirring
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Abstract
The present invention provides a kind of rubber adhesives and preparation method thereof, belong to adhesive preparing technical field.It solves the problems such as existing adhesive RC adhesive properties are poor, and preparation process is complicated.The present invention includes White Carbon black and adhesive A B 30, and the mass ratio of White Carbon black and adhesive A B 30 are 2：(2.5 3.5), adhesive A B 30 include bisphenol-A and adhesive A, and the mass ratio of bisphenol-A and adhesive A is 9：(18 22), adhesive A include methanol, hexamethylolmelamine, the concentrated sulfuric acid and lye, methanol, hexamethylolmelamine, the concentrated sulfuric acid and lye mass percent be respectively 63% 69%, 31% 35%, 0.1% 1% and 0.4% 1%.The present invention includes the preparation of adhesive A, the preparation of adhesive A B 30.Preparation method of the present invention is easy to operate, efficient, and the product obtained is uniformly dispersed, and prevented from caking, performance is good.
Description
Technical field
The invention belongs to adhesive preparing technical field, more particularly to a kind of rubber adhesive and preparation method thereof.
Background technology
The coherent medium of solid material surface of the same race or not of the same race can be referred to as adhesive, also referred to as glue
Glutinous agent is called bonding or glue by the method that the bonding force of adhesive makes the surface of solids connect.
Adhesive RC has both formaldehyde donor and formaldehyde acceptor dual function, and between category, first, white binding system is suitable for
The bonding of various rubber and framework material, including with the framework materials such as coppered steel wire, polyester, be also especially suitable for fluorubber and sail
The bonding of cloth, nylon and aramid fiber.
Existing adhesive RC adhesive properties are poor, and its preparation process is more complex, the product lack of homogeneity and appearance of preparation
Easily caking.
Invention content
The purpose of the present invention is for the disadvantages mentioned above present in existing adhesive RC, and provide a kind of rubber adhesive and
Preparation method, the preparation method is easy to operate, efficient, and the product obtained is uniformly dispersed, prevented from caking, performance
It is good.
Object of the invention can be realized by the following technical scheme：
A kind of rubber adhesive, which is characterized in that it includes White Carbon black and adhesive A B-30, the White Carbon black with it is viscous
The mass ratio of mixture AB-30 is 2：(2.5-3.5), the adhesive A B-30 include bisphenol-A and adhesive A, and described is double
The mass ratio of phenol A and adhesive A is 9：(18-22), the adhesive A include methanol, hexamethylolmelamine, dense sulphur
Acid and alkali liquid, the methanol, hexamethylolmelamine, the concentrated sulfuric acid and lye mass percent be respectively 63%-69%,
31%-35%, 0.1%-1% and 0.4%-1%.
Preferably, the mass fraction of the methanol is 98%.
Preferably, the mass fraction of the concentrated sulfuric acid is 98%.
A kind of preparation method of rubber adhesive, which is characterized in that it includes the following steps：
Step 1：The preparation 1. of adhesive A weighs, feeds intake, stirs and weighs 63%-69% first by above-mentioned mass percent
The methanol weighed is added for alcohol, 31%-35% hexamethylolmelamines, the 0.1%-1% concentrated sulfuric acids and 0.4%-1% lye
It into reaction kettle A, starts blender and is stirred, the hexamethylolmelamine weighed is added；2. 0.1%-1% is added in etherificate
It is 2-3 that the concentrated sulfuric acid, which adjusts pH value, and heating, it is 40 DEG C -65 DEG C to make the temperature in reaction kettle A, and etherification reaction occurs, and keeps the temperature 1h-
1.5h obtains ether-based liquid；3. lye is added in alkalization, tune pH value is 8-9；4. concentration purification squeezes into the ether-based liquid in reaction kettle A dense
Contracting tank, carries out concentration purification, starts vacuum pump, and remaining methanol and moisture, wait for vacuum degree -0.092MPa in extraction kettle A
More than, when temperature rises to 100 DEG C -120 DEG C, keep the temperature 1.3h-1.7h；5. outlet valve is opened in filtering, the object in reaction kettle A is released
Material, filtering obtain finished product adhesive A, storage.
The preparation 1. of step 2 adhesive A B-30 weighs, stirring, heats and press mass ratio 9：(18-22) weigh bisphenol-A and
Above-mentioned adhesive A all pours into the adhesive A weighed in reaction kettle B, when being heated with stirring to 55 DEG C -65 DEG C, by bisphenol-A point
Batch is added in reaction kettle B, after bisphenol-A is all added, the temperature in reaction kettle B is adjusted to 79 DEG C -81 DEG C, keeps the temperature 6h-7h；
2. cooling stops stirring, blowing makes feed liquid cool down, until feed liquid is fully crystallized white waxy solid；3. broken consolidate White waxy
Body, which pours into pulverizer, is ground into fritter shape adhesive A B-30 products.
Prepared by step 3 rubber adhesive of the present invention 1. weighs, feeds intake, stirring and weigh White Carbon black and adhesive A B-30, makes
The mass ratio of the two is 2：(2.5-3.5), White Carbon black vacuum suck stirring mixer after filtering start blender progress
Stirring would be heated in 88 DEG C -93 DEG C of adhesive A B-30 indentation stirring mixers, after the completion of charging, stir 1.2h-1.8h；
2. after mixing, blowing obtains the target product rubber adhesive of the present invention by three-dimensional reciprocating sieve sieving.
Preferably, the bisphenol-A in the step two is added in three times in reaction kettle B, is added within 8-12 minutes per minor tick
Enter.
Preferably, it in the step two, is discharged in stainless steel disc, naturally cools to the 2nd day, feed liquid, which is fully crystallized, is in
White waxy solid.
Preferably, the adhesive A B-30 for being heated to 88 DEG C -93 DEG C is to be pressurized to 0.1Mpa or more with air compressor machine,
It is pressed into stirring mixer.
Compared with prior art, preparation method of the present invention is easy to operate, efficient, and the product obtained is uniformly dispersed, no
Easily caking, performance are good.
Specific implementation mode
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
Preparing for rubber adhesive -1 is as follows：
The preparation 1. of step 1 adhesive A weighs, feeds intake, stirs and weighs 66% methanol, 33% by above-mentioned mass percent
Hexamethylolmelamine, 0.3% concentrated sulfuric acid and 0.7% lye, the methanol weighed is added in reaction kettle A, starts stirring
Machine is stirred, and the hexamethylolmelamine weighed is added；2. it is 2-3 that etherificate, which is added 0.3% concentrated sulfuric acid and adjusts pH value, add
Heat, it is 50 DEG C to make the temperature in reaction kettle A, and etherification reaction occurs, and heat preservation 1.3h obtains ether-based liquid；3. lye is added in alkalization, adjust
PH value is 8-9；4. the ether-based liquid (mixed liquor i.e. after etherification reaction in reaction kettle A, similarly hereinafter) in reaction kettle A is beaten in concentration purification
Enter concentration tank, carry out concentration purification, start vacuum pump, remaining methanol and moisture, wait for vacuum degree-in extraction kettle A
0.092MPa or more when temperature rises to 110 DEG C, keeps the temperature 1.5h；5. outlet valve is opened in filtering, the material in reaction kettle A, mistake are released
Filter obtains finished product adhesive A, storage.
The preparation 1. of step 2 adhesive A B-30 weighs, stirring, heats and press mass ratio 9：20 weigh bisphenol-A and above-mentioned
Adhesive A all pours into the adhesive A weighed in reaction kettle B, and when being heated with stirring to 60 DEG C, bisphenol-A is added in batches
In reaction kettle B (bisphenol-A is added in three times in reaction kettle B in the present embodiment, is added within 10 minutes per minor tick), bisphenol-A is whole
After addition, the temperature in reaction kettle B is adjusted to 80 DEG C, keeps the temperature 6.5h；2. cooling stops stirring, blowing makes feed liquid cool down, until material
Liquid is fully crystallized white waxy solid and (in the present embodiment, is discharged in stainless steel disc, naturally cools to the 2nd day, feed liquid is complete
Crystallize white waxy solid)；3. broken pour into white waxy solid in pulverizer is ground into the B-30 productions of fritter shape adhesive A
Product.
Prepared by step 3 rubber adhesive of the present invention 1. weighs, feeds intake, stirring and weigh White Carbon black and adhesive A B-30, makes
The mass ratio of the two is 2：3, White Carbon black vacuum suck stirring mixer after filtering starts blender and is stirred, will
It is heated to 90 DEG C of adhesive A B-30 to be pressurized in 0.1Mpa or more indentation stirring mixers with air compressor machine, after the completion of charging, stir
Mix 1.5h；2. after mixing, blowing obtains the target product rubber adhesive of the present invention by three-dimensional reciprocating sieve sieving.
Embodiment 2
Preparing for rubber adhesive -2 is as follows：
The preparation 1. of step 1 adhesive A weighs, feeds intake, stir by above-mentioned mass percent weigh 63.5% methanol,
35% hexamethylolmelamine, 0.5% concentrated sulfuric acid and 1% lye, the methanol weighed is added in reaction kettle A, starts and stirs
The machine of mixing is stirred, and the hexamethylolmelamine weighed is added；2. it is 2-3 that etherificate, which is added 5% concentrated sulfuric acid and adjusts pH value, add
Heat, it is 40 DEG C to make the temperature in reaction kettle A, and etherification reaction occurs, and heat preservation 1h obtains ether-based liquid；3. lye is added in alkalization, PH is adjusted
Value is 8-9；4. the ether-based liquid in reaction kettle A is squeezed into concentration tank by concentration purification, concentration purification is carried out, starts vacuum pump, extraction
Remaining methanol and moisture in reaction kettle A, wait for vacuum degree -0.092MPa or more, when temperature rises to 100 DEG C, keep the temperature 1.3h；5. mistake
Outlet valve is opened in filter, releases the material in reaction kettle A, and filtering obtains finished product adhesive A, storage.
The preparation 1. of step 2 adhesive A B-30 weighs, stirring, heats and press mass ratio 9：18 weigh bisphenol-A and above-mentioned
Adhesive A all pours into the adhesive A weighed in reaction kettle B, and when being heated with stirring to 55 DEG C, bisphenol-A is added in batches
In reaction kettle B (bisphenol-A is added in three times in reaction kettle B in the present embodiment, is added within 8 minutes per minor tick), bisphenol-A all adds
After entering, the temperature in reaction kettle B is adjusted to 79 DEG C, keeps the temperature 6h；2. cooling stops stirring, blowing makes feed liquid cool down, until feed liquid is complete
The white waxy solid of holocrystalline (in the present embodiment, is discharged in stainless steel disc, naturally cools to the 2nd day, feed liquid is fully crystallized
White waxy solid)；3. broken pour into white waxy solid in pulverizer is ground into fritter shape adhesive A B-30 products.
Prepared by step 3 rubber adhesive of the present invention 1. weighs, feeds intake, stirring and weigh White Carbon black and adhesive A B-30, makes
The mass ratio of the two is 2：2.5, White Carbon black vacuum suck stirring mixer after filtering starts blender and is stirred,
88 DEG C of adhesive A B-30 is would be heated to be pressurized in 0.1Mpa or more indentation stirring mixers with air compressor machine, after the completion of charging,
Stir 1.2h；2. after mixing, blowing obtains the target product rubber adhesive of the present invention by three-dimensional reciprocating sieve sieving.
Embodiment 3
Preparing for rubber adhesive -3 is as follows：
The preparation 1. of step 1 adhesive A weighs, feeds intake, stir by above-mentioned mass percent weigh 68.5% methanol,
31% hexamethylolmelamine, 0.1% concentrated sulfuric acid and 0.4% lye, the methanol weighed is added in reaction kettle A, is started
Blender is stirred, and the hexamethylolmelamine weighed is added；It is 2-3 that 2. etherificate, which is added 0.1% concentrated sulfuric acid and adjusts pH value,
Heating, it is 65 DEG C to make the temperature in reaction kettle A, and etherification reaction occurs, and heat preservation 1.5h obtains ether-based liquid；3. lye is added in alkalization,
Tune pH value is 8-9；4. the ether-based liquid in reaction kettle A is squeezed into concentration tank by concentration purification, concentration purification is carried out, starts vacuum pump,
Remaining methanol and moisture in extraction kettle A, wait for vacuum degree -0.092MPa or more, when temperature rises to 120 DEG C, keep the temperature 1.7h；
5. outlet valve is opened in filtering, the material in reaction kettle A is released, filtering obtains finished product adhesive A, storage.
The preparation 1. of step 2 adhesive A B-30 weighs, stirring, heats and press mass ratio 9：22 weigh bisphenol-A and above-mentioned
The adhesive A weighed, is all poured into reaction kettle B that (bisphenol-A is added to reaction kettle B in three times in the present embodiment by adhesive A
In, it is added within 12 minutes per minor tick), when being heated with stirring to 65 DEG C, bisphenol-A is added in batches in reaction kettle B, bisphenol-A is complete
After portion is added, the temperature in reaction kettle B is adjusted to 81 DEG C, keeps the temperature 7h；2. cooling stops stirring, blowing makes feed liquid cool down, until material
Liquid is fully crystallized white waxy solid and (in the present embodiment, is discharged in stainless steel disc, naturally cools to the 2nd day, feed liquid is complete
Crystallize white waxy solid)；3. broken pour into white waxy solid in pulverizer is ground into the B-30 productions of fritter shape adhesive A
Product.
Prepared by step 3 rubber adhesive of the present invention 1. weighs, feeds intake, stirring and weigh White Carbon black and adhesive A B-30, makes
The mass ratio of the two is 2：3.5, White Carbon black vacuum suck stirring mixer after filtering starts blender and is stirred,
93 DEG C of adhesive A B-30 is would be heated to be pressurized in 0.1Mpa or more indentation stirring mixers with air compressor machine, after the completion of charging,
Stir 1.8h；2. after mixing, blowing obtains the target product rubber adhesive of the present invention by three-dimensional reciprocating sieve sieving.
It should be understood that in claims of the present invention, specification, all " including ... " should be understood as open
Meaning, that is, its meaning is equal to " at least containing ... ", and should not be construed as enclosed meaning, i.e., its meaning is not answered
This is interpreted as " only including ... ".
Those skilled in the art can make various modifications to described specific embodiment
Or supplement or substitute by a similar method, however, it does not deviate from the spirit of the invention or surmounts the appended claims determines
The range of justice.
Claims (7)
1. a kind of rubber adhesive, which is characterized in that it includes White Carbon black and adhesive A B-30, the White Carbon black and bonding
The mass ratio of agent AB-30 is 2：(2.5-3.5), the adhesive A B-30 include bisphenol-A and adhesive A, the bis-phenol
The mass ratio of A and adhesive A is 9：(18-22), the adhesive A include methanol, hexamethylolmelamine, the concentrated sulfuric acid
And lye, the methanol, hexamethylolmelamine, the concentrated sulfuric acid and lye mass percent be respectively 63%-69%,
31%-35%, 0.1%-1% and 0.4%-1%.
2. a kind of rubber adhesive according to claim 1, which is characterized in that the mass fraction of the methanol is
98%.
3. a kind of rubber adhesive according to claim 1 or 2, which is characterized in that the mass fraction of the concentrated sulfuric acid
It is 98%.
4. a kind of preparation method of rubber adhesive, is used to prepare rubber adhesive as described in claim 1, feature exists
In it includes the following steps：
The preparation 1. of step 1 adhesive A weighs, feeds intake, stir by above-mentioned mass percent weigh 63%-69% methanol,
31%-35% hexamethylolmelamines, the 0.1%-1% concentrated sulfuric acids and 0.4%-1% lye, the methanol weighed is added to instead
It answers in kettle A, starts blender and be stirred, the hexamethylolmelamine weighed is added；2. the dense sulphur of 0.1%-1% is added in etherificate
It is 2-3 that acid, which adjusts pH value, and heating, it is 40 DEG C -65 DEG C to make the temperature in reaction kettle A, and etherification reaction occurs, and heat preservation 1h-1.5h is obtained
Obtain ether-based liquid；3. lye is added in alkalization, tune pH value is 8-9；4. the ether-based liquid in reaction kettle A is squeezed into concentration tank by concentration purification,
It carrying out concentration purification, starts vacuum pump, remaining methanol and moisture, wait for vacuum degree -0.092MPa or more in extraction kettle A,
When temperature rises to 100 DEG C -120 DEG C, 1.3h-1.7h is kept the temperature；5. outlet valve is opened in filtering, the material in reaction kettle A, mistake are released
Filter obtains finished product adhesive A, storage；
The preparation 1. of step 2 adhesive A B-30 weighs, stirring, heats and press mass ratio 9：(18-22) weighs bisphenol-A and above-mentioned
Adhesive A all pours into the adhesive A weighed in reaction kettle B, when being heated with stirring to 55 DEG C -65 DEG C, in batches by bisphenol-A
It is added in reaction kettle B, after bisphenol-A is all added, the temperature in reaction kettle B is adjusted to 79 DEG C -81 DEG C, keeps the temperature 6h-7h；2. cold
But stop stirring, blowing makes feed liquid cool down, until feed liquid is fully crystallized white waxy solid；3. broken fall white waxy solid
Enter to be ground into fritter shape adhesive A B-30 products in pulverizer；
Prepared by step 3 rubber adhesive 1. weighs, feeds intake, stirring and weigh White Carbon black and adhesive A B-30, makes the quality of the two
The ratio between be 2：(2.5-3.5), White Carbon black vacuum suck stirring mixer after filtering start blender and are stirred, and will add
In heat to 88 DEG C -93 DEG C of adhesive A B-30 indentation stirring mixers, after the completion of charging, 1.2h-1.8h is stirred；2. mixing is equal
After even, blowing obtains the target product rubber adhesive of the present invention by three-dimensional reciprocating sieve sieving.
5. a kind of preparation method of rubber adhesive according to claim 4, which is characterized in that in the step two
Bisphenol-A is added in three times in reaction kettle B, is added within 8-12 minutes per minor tick.
6. a kind of preparation method of rubber adhesive according to claim 4, which is characterized in that in the step two,
It is discharged in stainless steel disc, naturally cools to the 2nd day, feed liquid is fully crystallized white waxy solid.
7. a kind of preparation method of rubber adhesive according to claim 4, which is characterized in that described is heated to 88
DEG C -93 DEG C of adhesive A B-30 is to be pressurized to 0.1Mpa or more with air compressor machine, is pressed into stirring mixer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810359669.8A CN108624269A (en) | 2018-04-20 | 2018-04-20 | A kind of rubber adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810359669.8A CN108624269A (en) | 2018-04-20 | 2018-04-20 | A kind of rubber adhesive and preparation method thereof |
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| Publication Number | Publication Date |
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| CN108624269A true CN108624269A (en) | 2018-10-09 |
Family
ID=63694135
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| CN201810359669.8A Pending CN108624269A (en) | 2018-04-20 | 2018-04-20 | A kind of rubber adhesive and preparation method thereof |
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| KR100188810B1 (en) * | 1997-03-19 | 1999-06-01 | 홍건희 | Rubber composition for tire cord having good water-resistant adhesion property |
| CN101817913A (en) * | 2010-03-11 | 2010-09-01 | 浙江奥仕化学有限公司 | Preparation method of highly methyl etherified amino resin |
| CN102002329A (en) * | 2010-09-30 | 2011-04-06 | 泰州五行消防水带有限公司 | Binding agent for composite material of hydrogenated nitrile rubber and para-aramid fiber and preparation method thereof |
| CN101691474B (en) * | 2009-08-27 | 2011-08-17 | 招远市鹏泰轮胎翻新有限公司 | Tire procuring in-plastic-mat in large project and preparation method thereof |
| CN103086992A (en) * | 2012-11-14 | 2013-05-08 | 江苏国立化工科技有限公司 | Preparation method of hexamethoxymethyl melamine resin |
| CN103602288A (en) * | 2013-12-11 | 2014-02-26 | 五行材料科技（江苏）有限公司 | Rubber solid adhesive, and preparation method and application thereof |
| CN106349444A (en) * | 2016-08-25 | 2017-01-25 | 江苏国立化工科技有限公司 | Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) |
| CN106349985A (en) * | 2016-08-25 | 2017-01-25 | 江苏国立化工科技有限公司 | Preparation method of rubber adhesive RA65 |
-
2018
- 2018-04-20 CN CN201810359669.8A patent/CN108624269A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58126151A (en) * | 1982-01-25 | 1983-07-27 | 株式会社明治ゴム化成 | Composite material consisting of rubber and metal and its manufacture |
| KR100188810B1 (en) * | 1997-03-19 | 1999-06-01 | 홍건희 | Rubber composition for tire cord having good water-resistant adhesion property |
| CN101691474B (en) * | 2009-08-27 | 2011-08-17 | 招远市鹏泰轮胎翻新有限公司 | Tire procuring in-plastic-mat in large project and preparation method thereof |
| CN101817913A (en) * | 2010-03-11 | 2010-09-01 | 浙江奥仕化学有限公司 | Preparation method of highly methyl etherified amino resin |
| CN102002329A (en) * | 2010-09-30 | 2011-04-06 | 泰州五行消防水带有限公司 | Binding agent for composite material of hydrogenated nitrile rubber and para-aramid fiber and preparation method thereof |
| CN103086992A (en) * | 2012-11-14 | 2013-05-08 | 江苏国立化工科技有限公司 | Preparation method of hexamethoxymethyl melamine resin |
| CN103602288A (en) * | 2013-12-11 | 2014-02-26 | 五行材料科技（江苏）有限公司 | Rubber solid adhesive, and preparation method and application thereof |
| CN106349444A (en) * | 2016-08-25 | 2017-01-25 | 江苏国立化工科技有限公司 | Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) |
| CN106349985A (en) * | 2016-08-25 | 2017-01-25 | 江苏国立化工科技有限公司 | Preparation method of rubber adhesive RA65 |
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