CN103030838A - Silane coupling agent and preparation thereof - Google Patents
Silane coupling agent and preparation thereof Download PDFInfo
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- CN103030838A CN103030838A CN2013100147336A CN201310014733A CN103030838A CN 103030838 A CN103030838 A CN 103030838A CN 2013100147336 A CN2013100147336 A CN 2013100147336A CN 201310014733 A CN201310014733 A CN 201310014733A CN 103030838 A CN103030838 A CN 103030838A
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- silane coupling
- terephthalic acid
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Abstract
The invention relates to silane coupling agent which comprises terephthalic acid metal salt, silane coupling agent, stearic acid and white carbon black. The invention further provides a preparation method for the silane coupling agent: the activation of the power is implemented firstly, that is, terephthalic acid metal salt powder becomes surface-oleophylic from surface-hydrophilic after activating agent stearic acid treatment. The method comprises the following specific steps: the terephthalic acid metal salt and the stearic acid are added into a stirring kettle and stirred for 5 minutes at the speed of 2000 r/min, and stirring is stopped for 15-minute activation; then the white carbon black is added to mix, and is stirred for 10 minutes at the speed of 2000 r/min; and then the silane coupling agent is added at the constant speed to continuously stir for 10 minutes at the speed of 2000 r/min to obtain the finished product. The silane coupling agent has excellent performance, good compatibility with rubber and anti-sulfur reversion effect, can effectively improve the compatibility of inorganic powder, such as the white carbon black and the like with the rubber, and can reduce the user cost.
Description
Technical field
The present invention relates to a kind of rubber silane coupling agent.
Background technology
Coupling agent refers to improve the chemical substance of bonding force between inorganic reinforcement or filler and polymer interface, is commonly used for the surface-modifying agent of inorganic powder material.Divide by chemical structure, coupling agent mainly contains silicane, titanate ester, P contained compound class, amine and complex compound class.Wherein, silane coupling agent is a kind of that kind is maximum now, consumption is maximum.Yet mostly there is a problem in silane coupling agent, and namely silane coupling agent generally is transparent liquid, meets water or can be hydrolyzed when contact with moisture, brings very big inconvenience to its transportation, use.Each company has proposed different improvement projects one after another for addressing this problem.Nanjing dawn Chemical Group obtains black solid coupling agent Si69C with regard to two-(the silica-based propyl group of γ-triethoxy) tetrasulfide Si69 is mixed with 1: 1 ratio with carbon black, substitutes the consumption of Si69 portion with two parts consumptions.This product has solved the problem of Si69 transportation, weighing inconvenience.But it has certain limitation in application, namely is not suitable for light color and colour product is arranged.
Terephthalic acid is called for short PTA, is the di-carboxylic acid of output maximum, mainly makes from p-Xylol, is the main raw material of producing polyester.Publication number is that the Chinese invention patent application of CN1283607A discloses a kind of phthalic acid rare earth, by will, adjacent, m-phthalic acid or phthalate anhydride saponification being replaced through rare earth salts again, can do thermo-stabilizer, also can be used as coupling agent.Yet the China rare earth reserves have slumped 37% between 1996 to 2009, only surplus 2,700 ten thousand tons.By existing production rate, in China, heavy class rare earth deposit only can keep 15 to 20 years.
Summary of the invention
Purpose of the present invention to provide exactly a kind of efficient, nontoxic, cheap, preparation technology is simple, can effectively solve the problem of silane coupling agent transportation, weighing, be applicable to light color and the coupling agent substitute of colour product is arranged, can improve again the coupling agent of the processing characteristics of rubber.
The technical scheme that realizes the object of the invention is:
A kind of novel silane coupler, it consists of: terephthaldehyde's acid metal salt 40-60 part, silane coupling agent 35-50 part, stearic acid 1-3 part, white carbon black 3-10 part.
In the preferred terephthalic acid calcium of described terephthaldehyde's acid metal salt, terephthalic acid magnesium, terephthalic acid zinc, potassium terephthalate, para-phthalic sodium, terephthalic acid barium, terephthalic acid aluminium, the terephthalic acid iron one or more.
Described silane coupling agent can be one or more in γ-r-chloropropyl trimethoxyl silane (KH-792), two-(the silica-based propyl group of γ-triethoxy) tetrasulfide (Si69), two (the silica-based propyl group of triethoxy) disulphide (Si75), gamma-mercaptopropyltriethoxysilane (KH-580), γ-aminopropyl triethoxysilane (KH-550), γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane (KH-560).
A kind of method for preparing novel silane coupler: at first carry out the activation of powder, being about to becomes surperficial oleophylic after terephthalic acid metal-salt powder is processed by activated dose of stearic acid of surface hydrophilic.Concrete grammar for terephthaldehyde's acid metal salt and stearic acid are added jointly stirring tank (2000 turn/ speed in min) stirs 5min, stops and activate 15min.Add again white carbon black and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds silane coupling agent again, continue with 2000 turn/min speed stirs 10min, namely gets the present invention.
The advantage of the invention: technique of the present invention is simple, and the products obtained therefrom excellent property is good with rubber compatibility, but the consistency of the inorganic powder such as Effective Raise white carbon black and rubber.Have anti-sulfuration and return unit's effect, can reduce user cost.
Description of drawings
Compressing tablet figure after the coupling agent that Fig. 1: embodiment 1 makes, white carbon black and natural rubber are mixing
Compressing tablet figure after the coupling agent that Fig. 2: embodiment 2 makes, white carbon black and natural rubber are mixing
Compressing tablet figure after the coupling agent that Fig. 3: embodiment 3 makes, white carbon black and natural rubber are mixing
Compressing tablet figure after the coupling agent that Fig. 4: embodiment 4 makes, white carbon black and natural rubber are mixing
Compressing tablet figure after the coupling agent that Fig. 5: embodiment 5 makes, white carbon black and natural rubber are mixing
Compressing tablet figure after the coupling agent that Fig. 6: embodiment 6 makes, white carbon black and natural rubber are mixing
Compressing tablet figure after the coupling agent that Fig. 7: embodiment 7 makes, white carbon black and natural rubber are mixing
Fig. 8: the compressing tablet figure after white carbon black and natural rubber are mixing
Compressing tablet figure after Fig. 9: Si69, white carbon black and natural rubber are mixing
Embodiment
Embodiment 1
40 parts of terephthalic acid calcium and 2 parts of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 8 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 50 parts of silane coupling agent KH-792 again, continue with 2000 turn/min speed stirs 10min, namely gets sample 1 of the present invention.
Embodiment 2
30 parts of terephthalic acid calcium, 30 parts of terephthalic acid zinc and 1 part of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 4 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 35 parts of silane coupling agent Si69 again, continue with 2000 turn/min speed stirs 10min, namely gets sample 2 of the present invention.
Embodiment 3
44 parts of terephthalic acid magnesium and 3 parts of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 10 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 43 parts of silane coupling agent Si75 again, continue with 2000 turn/min speed stirs 10min, namely gets sample 3 of the present invention.
Embodiment 4
45 parts to terephthalic acid zinc and 2 parts of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 3 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 40 parts of silane coupling agent KH-580 again, continue with 2000 turn/min speed stirs 10min, namely gets sample 4 of the present invention.
Embodiment 5
25 parts of potassium terephthalates, 25 parts of para-phthalic sodiums and 3 parts of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 7 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 40 parts of silane resin acceptor kh-550s again, continue with 2000 turn/min speed stirs 10min, namely gets sample 5 of the present invention.
Embodiment 6
15 parts of terephthalic acid barium, 20 parts of terephthalic acid aluminium, 20 parts of terephthalic acid iron and 3 parts of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 5 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 37 parts of silane coupling agent KH-560 again, continue with 2000 turn/min speed stirs 10min, namely gets sample 6 of the present invention.
Embodiment 7
25 parts of terephthalic acid calcium, 25 parts of terephthalic acid magnesium and 3 parts of stearic acid jointly add stirring tank (2000 turn/ speed in min) stirs 5min, stops activation 15min.Add again 7 parts of white carbon blacks and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds 40 parts of silane coupling agent Si69 again, continue with 2000 turn/min speed stirs 10min, namely gets sample 7 of the present invention.
Embodiment 8
Dispersing property test: sample 1-7, common silane coupling agent Si6920 part and 40 parts of white carbon blacks are added in 100 parts of rubber the impact of test dialogue carbon black dispersion performance.
Physical and mechanical properties: in 5 parts of coupling agents, 5 parts in zinc oxide, 1.0 parts in sulphur, 100 parts of rubber of 0.6 part of adding of accelerant CZ, film-making is measured index in 143 ℃ of sulfuration 60min over cure situations.The detection of 300% stress at definite elongation (adopting GB/T8656); The detection of tensile strength and tensile yield (adopting GB/T8656)
Find out that from accompanying drawing gained white carbon black filler of the present invention is than traditional white carbon black filler, its dispersing property in rubber is very good, can not produce large-sized aggregate.
As can be seen from the table, compare with Si69 and blank sample, the stress at definite elongation of gained sample and tensile strength increase, tensile yield reduces, this shows that in sulfidation product of the present invention has played the effect of recovery agent, has compensated the loss of rubber cross density.
Take above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, the relevant staff can in the scope that does not depart from this invention technological thought, carry out various change and modification fully.The technical scope of this invention is not limited to the content on the specification sheets, must determine its technical scope according to the claim scope.
Claims (5)
1. a silane coupling agent is characterized in that: contain terephthaldehyde's acid metal salt, silane coupling agent, stearic acid and white carbon black.
2. silane coupling agent as claimed in claim 1 is characterized in that: terephthaldehyde's acid metal salt 40-60 part, silane coupling agent 35-50 part, stearic acid 1-3 part, white carbon black 3-10 part.
3. silane coupling agent as claimed in claim 2 is characterized in that: one or more in the preferred terephthalic acid calcium of described terephthaldehyde's acid metal salt, terephthalic acid magnesium, terephthalic acid zinc, potassium terephthalate, para-phthalic sodium, terephthalic acid barium, terephthaldehyde's lead plumbate, terephthalic acid aluminium, the terephthalic acid iron.
4. silane coupling agent as claimed in claim 1, it is characterized in that: described silane coupling agent can be one or more in γ-r-chloropropyl trimethoxyl silane (KH-792), two-(the silica-based propyl group of γ-triethoxy) tetrasulfide (Si69), two (the silica-based propyl group of triethoxy) disulphide (Si75), gamma-mercaptopropyltriethoxysilane (KH-580), γ-aminopropyl triethoxysilane (KH-550), γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane (KH-560).
5. such as the preparation method of claim 1 to 4 silane coupling agent as described in each, it is characterized in that: at first carry out the activation of powder, being about to becomes surperficial oleophylic after terephthalic acid metal-salt powder is processed by activated dose of stearic acid of surface hydrophilic.Concrete grammar for terephthaldehyde's acid metal salt and stearic acid are added jointly stirring tank (2000 turn/ speed in min) stirs 5min, stops and activate 15min.Add again white carbon black and mix, with 2000 turn/min speed stirs 10min, at the uniform velocity adds silane coupling agent again, continue with 2000 turn/min speed stirs 10min, obtains finished product.
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| CN2013100147336A CN103030838A (en) | 2013-01-16 | 2013-01-16 | Silane coupling agent and preparation thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072823A (en) * | 2014-07-09 | 2014-10-01 | 常州市五洲化工有限公司 | Rubber antiager |
| CN104072802A (en) * | 2014-07-09 | 2014-10-01 | 常州市五洲化工有限公司 | Silane coupling agent |
| CN104086803A (en) * | 2014-07-09 | 2014-10-08 | 常州市五洲化工有限公司 | Rubber anti-aging agent |
| CN105778155A (en) * | 2016-05-12 | 2016-07-20 | 上海橡瑞新材料科技有限公司 | Anti-aging agent NBC coated with nanomaterial and preparation method of anti-aging agent NBC |
| CN107419255A (en) * | 2017-07-27 | 2017-12-01 | 泾县信达工贸有限公司 | A kind of aluminium alloy electric hot plate processing method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061012A (en) * | 2010-12-07 | 2011-05-18 | 江苏爱特恩高分子材料有限公司 | Novel silane coupling agent and preparation method thereof |
| CN102585294A (en) * | 2012-01-12 | 2012-07-18 | 江苏爱特恩高分子材料有限公司 | Compound rubber bonding promoting agent and preparation method thereof |
-
2013
- 2013-01-16 CN CN2013100147336A patent/CN103030838A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061012A (en) * | 2010-12-07 | 2011-05-18 | 江苏爱特恩高分子材料有限公司 | Novel silane coupling agent and preparation method thereof |
| CN102585294A (en) * | 2012-01-12 | 2012-07-18 | 江苏爱特恩高分子材料有限公司 | Compound rubber bonding promoting agent and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072823A (en) * | 2014-07-09 | 2014-10-01 | 常州市五洲化工有限公司 | Rubber antiager |
| CN104072802A (en) * | 2014-07-09 | 2014-10-01 | 常州市五洲化工有限公司 | Silane coupling agent |
| CN104086803A (en) * | 2014-07-09 | 2014-10-08 | 常州市五洲化工有限公司 | Rubber anti-aging agent |
| CN104072823B (en) * | 2014-07-09 | 2016-03-23 | 常州市五洲化工有限公司 | A kind of rubber antioxidant |
| CN104086803B (en) * | 2014-07-09 | 2016-06-01 | 常州市五洲化工有限公司 | A kind of rubber anti-ageing agent |
| CN105778155A (en) * | 2016-05-12 | 2016-07-20 | 上海橡瑞新材料科技有限公司 | Anti-aging agent NBC coated with nanomaterial and preparation method of anti-aging agent NBC |
| CN105778155B (en) * | 2016-05-12 | 2019-04-19 | 上海橡瑞新材料科技有限公司 | A kind of antioxidant NBC and preparation method thereof coating nano material |
| CN107419255A (en) * | 2017-07-27 | 2017-12-01 | 泾县信达工贸有限公司 | A kind of aluminium alloy electric hot plate processing method |
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Application publication date: 20130410 |