CN101759860B - Production method for granular rubber aging inhibitor FR - Google Patents
Production method for granular rubber aging inhibitor FR Download PDFInfo
- Publication number
- CN101759860B CN101759860B CN2009102282302A CN200910228230A CN101759860B CN 101759860 B CN101759860 B CN 101759860B CN 2009102282302 A CN2009102282302 A CN 2009102282302A CN 200910228230 A CN200910228230 A CN 200910228230A CN 101759860 B CN101759860 B CN 101759860B
- Authority
- CN
- China
- Prior art keywords
- aging inhibitor
- gel
- under
- fluid
- diameter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a production method for a granular rubber aging inhibitor FR. In the method, the aging inhibitor FR is heated to form gel, the gel is input into a granulating pipe with the diameter of 0.2 to 5mm under the pressure of 0.2 to 1MPa, a fluid is controlled within the range of smooth flow, disturbance with the frequency of 50 to 500Hz is carried out on the fluid so as to crack the fluid and form uniform liquid drops, and then the liquid drops are crystallized and solidified in the falling process so as to form the granular rubber aging inhibitor FR with uniform granularity. The advantages of the production method are as follows: the operation of the new process is simple; being uniform granules, the inhibitor FR cannot be easily crushed; dust pollution is avoided in the manufacturing and using processes; the automatic weighing can be realized; moreover, the inhibitor FR has good fluidity and dispersibility.
Description
Technical field
The present invention relates to a kind of high-content rubber antioxidant 2,2,4-trimethylammonium-1, the working method of 2-dihyaroquinoline polymkeric substance (FR) belongs to the rubber aging inhibitor FR production technical field.
Background technology
The special-purpose aging inhibitor FR of automobile radial is one type of outstanding especially universal anti-aging agent of anti ageing property in the rubber industry, is widely used in various tires, sebific duct, adhesive tape and other rubber item.The FR product active constituent content low (effective constituent is dimer, tripolymer and the tetramer) that adopts traditional technology to produce at present; Can't satisfy the radial tyre production requirement; And because product generally is a sheet structure; It is mobile poor, easy to be broken to exist product, and dust pollution is serious in production, the use, can't realize a series of problems such as automatic gauge and homodisperse.Document (Chinese patent, application number: CN 200410070777.5) has been reported production high purity 2,2,4-trimethylammonium-1, and the method for 2-dihyaroquinoline polymkeric substance (FR) has adopted two-step approach to prepare FR.At first under the condition that acid exists, make aniline and acetone generation condensation reaction obtain mixture, separate obtaining 2 then; 2,4-trimethylammonium-1,2-dihyaroquinoline monomer; Under high-temperature low-pressure, use in the hydro carbons inert solvent with purging compound after repolymerization obtain 2; 2,4-trimethylammonium-1,2-dihyaroquinoline polymkeric substance.Two-step process is complicated, and production cost is high, and the finished product that obtain are sheet structure, and dust pollution is serious, and the flowability of product and bad dispersibility during use can't realize automatic weighing.Document (Speciality Petrochemicals, 2005,5:36) reported the technical study that one-step catalytic synthesizes aging inhibitor FR, the preferable reaction conditions that obtains: with BF
3Be catalyzer, BF
3/ aniline (mol ratio)=0.05: 1, acetone joining day 4h, aniline/acetone (mol ratio)=2.5: 1; Product has preferable quality, but ash content is higher, and because product also is a sheet structure; There are flowability and bad dispersibility equally, can't realize automatic weighing.Therefore, production technique is simple, in active constituent content height, good fluidity, the use dust pollution little, can realize that automatic gauge and homodisperse FR are the keys that realizes the FR widespread use.
Summary of the invention
The object of the present invention is to provide a kind of production technique of granular rubber aging inhibitor FR, this technological operation is simple, and the FR product prepn is become spherulitic, has solved dust pollution question, use has realized automatic weighing, flowability and good dispersivity.
For achieving the above object, the present invention realizes through following technical proposals: a kind of production technique of granular rubber aging inhibitor FR is characterized in that comprising following process:
1. aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 0.2～1MPa in the granulation pipe that diameter is 0.2～5mm; Fluid is controlled in the smooth flow scope, and it is 50～500 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby forms even-grained granular rubber aging inhibitor FR.
The invention has the advantages that: this novel process is simple to operate, and FR is a homogeneous spherulitic particle, is difficult for fragmentation, and no dust pollution in manufacturing and the use can be realized automatic weighing, has good flowability and dispersed.
Embodiment
Example 1:
Join 1mol aniline, 0.2mol toluene, 0.01mol catalyzer tosic acid in the reaction kettle successively; In temperature of reaction is that 90 ℃, rotating speed are under 500 rev/mins the condition; 1.5mol acetone is added drop-wise in the reaction kettle; Dropwise in 5 hours, acetone drips continued reaction 0.5 hour.Then, toluene distillation under normal pressure distills aniline under the condition of pressure for-0.02Mpa, obtain monomer.With the 0.5mol molar percentage is that 25% hydrochloric acid joins and contains in the monomeric reaction kettle, in temperature of reaction is under 70 ℃ the condition, to react 3 hours.With molar percentage is that 10% sodium hydroxide solution joins in the reaction kettle, and control Ph value is 8.5.Washing, granulation obtain product 2,2,4-trimethylammonium-1, and 2-dihyaroquinoline polymkeric substance, effective content are 80.2%.Above-mentioned aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 0.2MPa in the granulation pipe that diameter is 0.2mm; Fluid is controlled in the smooth flow scope, and it is 50 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby the formation diameter is 0.2mm, uniform granular rubber aging inhibitor FR.
Example 2:
The aging inhibitor FR that present embodiment adopted is identical with embodiment 1.Above-mentioned aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 0.6MPa in the granulation pipe that diameter is 2mm; Fluid is controlled in the smooth flow scope, and it is 250 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby the formation diameter is 2mm, uniform spherulitic high-content rubber aging inhibitor FR.
Example 3:
The aging inhibitor FR that present embodiment adopted is identical with embodiment 1.Above-mentioned aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 1MPa in the granulation pipe that diameter is 5mm; Fluid is controlled in the smooth flow scope, and it is 500 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby the formation diameter is 5mm, uniform spherulitic high-content rubber aging inhibitor FR.
Claims (1)
1. the working method of a granular rubber aging inhibitor FR; It is characterized in that comprising following process: join 1mol aniline, 0.2mol toluene, 0.01mol catalyzer tosic acid in the reaction kettle successively; In temperature of reaction is that 90 ℃, rotating speed are under 500 rev/mins the condition; 1.5mol acetone is added drop-wise in the reaction kettle, dropwises in 5 hours, acetone drips continued reaction 0.5 hour; Then, toluene distillation under normal pressure distills aniline under the condition of pressure for-0.02MPa, obtain monomer; With the 0.5mol molar percentage is that 25% hydrochloric acid joins and contains in the monomeric reaction kettle, in temperature of reaction is under 70 ℃ the condition, to react 3 hours; With molar percentage is that 10% sodium hydroxide solution joins in the reaction kettle, and control pH value is 8.5; Washing, granulation obtain product 2,2,4-trimethylammonium-1, and 2-dihyaroquinoline polymkeric substance, effective content are 80.2%; Above-mentioned aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 0.2MPa in the granulation pipe that diameter is 0.2mm; Fluid is controlled in the smooth flow scope, and it is 50 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby the formation diameter is 0.2mm, uniform granular rubber aging inhibitor FR; Perhaps above-mentioned aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 0.6MPa in the granulation pipe that diameter is 2mm; Fluid is controlled in the smooth flow scope, and it is 250 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby the formation diameter is 2mm, uniform granular rubber aging inhibitor FR; Perhaps above-mentioned aging inhibitor FR is added the thermosetting gel; Gel is imported under the pressure of 1MPa in the granulation pipe that diameter is 5mm; Fluid is controlled in the smooth flow scope, and it is 500 hertz disturbance that convection cell applies frequency, makes fluid break to form symmetrical liquid drop; Drop crystallization in dropping process is solidified, thereby the formation diameter is 5mm, uniform granular rubber aging inhibitor FR.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102282302A CN101759860B (en) | 2009-11-16 | 2009-11-16 | Production method for granular rubber aging inhibitor FR |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102282302A CN101759860B (en) | 2009-11-16 | 2009-11-16 | Production method for granular rubber aging inhibitor FR |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101759860A CN101759860A (en) | 2010-06-30 |
| CN101759860B true CN101759860B (en) | 2012-07-25 |
Family
ID=42491253
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102282302A Active CN101759860B (en) | 2009-11-16 | 2009-11-16 | Production method for granular rubber aging inhibitor FR |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101759860B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467372B (en) * | 2012-06-08 | 2015-09-09 | 中国石油化工股份有限公司 | The method of the combination producing of a kind of anti-aging agent RD and aging inhibitor FR |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046535A (en) * | 1990-05-05 | 1990-10-31 | 张绍文 | 2,2,4-trimethylammonium-1, the 2-dihyaroquinoline is polymeric-step-still method synthesis technique |
| US5126494A (en) * | 1988-01-11 | 1992-06-30 | Massachusetts Institute Of Technology | Methods for catalytic asymmetric dihydroxylation of olefins |
| CN101165086A (en) * | 2006-10-17 | 2008-04-23 | 泰安圣奥化工科技有限公司 | Spherical rubber auxiliary agent and preparation method thereof |
-
2009
- 2009-11-16 CN CN2009102282302A patent/CN101759860B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5126494A (en) * | 1988-01-11 | 1992-06-30 | Massachusetts Institute Of Technology | Methods for catalytic asymmetric dihydroxylation of olefins |
| CN1046535A (en) * | 1990-05-05 | 1990-10-31 | 张绍文 | 2,2,4-trimethylammonium-1, the 2-dihyaroquinoline is polymeric-step-still method synthesis technique |
| CN101165086A (en) * | 2006-10-17 | 2008-04-23 | 泰安圣奥化工科技有限公司 | Spherical rubber auxiliary agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101759860A (en) | 2010-06-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101134802A (en) | Novel process for synthesizing bead granular rubber antioxidant | |
| CN100575337C (en) | The method for preparing α-Qing Jibingxisuanzhi | |
| CN101580602A (en) | Production method of spherical high-content rubber antioxidant RD | |
| CN101759860B (en) | Production method for granular rubber aging inhibitor FR | |
| CN101817724B (en) | Preparation method of 1,2,4-trifluoro-benzene | |
| CN102382221B (en) | Phellandrene resin production process | |
| CN102079706A (en) | Synthesis method of hindered phenol antioxidant 1010 | |
| CN103553878B (en) | A kind of novel preparation method of cyclohexyl phenol class liquid crystal intermediates compound | |
| CN101591435A (en) | The production method of rubber aging inhibitor FR | |
| CN107486208B (en) | Preparation method and application of carbon nanotube-loaded quaternary amorphous nickel-based catalyst | |
| CN102702262B (en) | A kind of preparation method of melamine polyols phosphoric acid ester | |
| CN114058327A (en) | Special composite hot-melt pressure-sensitive adhesive for refrigerator back plate and preparation method thereof | |
| CN110776430B (en) | Preparation method of tri (2-aminoethyl) amine | |
| CN109019649B (en) | Preparation method of high-molecular-ratio potassium fluoroaluminate | |
| CN101898135A (en) | Amorphous catalyst for catalytic hydrogenation of 2-cyan-4-nitroaniline and preparation method of 2,5-diamincyanophenyl | |
| CN101367762B (en) | Preparation method of midbody 7-chloroquinaldine | |
| CN101168520A (en) | Method for producing 1,1'-phenylsulfonyl-4,4'-diallyl (2) ether | |
| CN112125846B (en) | Preparation method of 1, 7-di (9-acridinyl) heptane | |
| CN117363259B (en) | High-adhesive-strength tackifier and preparation method and application thereof | |
| CN111116319A (en) | Synthesis and refining method of high-purity 1, 6-dihydroxynaphthalene | |
| CN102702249B (en) | A kind of preparation method of isocyanuric acid polyolphosphateester | |
| CN103387519A (en) | Preparation method for 4-hydroxybenzyl cyanide | |
| CN115710159B (en) | Method for purifying 1-ethynyl cyclohexanol by using melt crystallization method | |
| CN114230548B (en) | Purification method of high-purity vinylene carbonate | |
| CN103408462B (en) | Industrial production method of 3-cyano-3,5,5-trimethylcyclohexanone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 300272 Tianjin City Haixin Binhai Industrial Zone Dagang Gulin Road No. 72 Patentee after: Kemai Chemical Co., Ltd. Address before: 300272, Grand Port, Tianjin Ancient Wood Street industrial and rural areas Patentee before: Tianjin Kemai Chemical Co., Ltd. |