CN103044328A - Synthesis of novel rubber vulcanizer 1, 1'-caprolactamdisulfide - Google Patents
Synthesis of novel rubber vulcanizer 1, 1'-caprolactamdisulfide Download PDFInfo
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- CN103044328A CN103044328A CN201210455766XA CN201210455766A CN103044328A CN 103044328 A CN103044328 A CN 103044328A CN 201210455766X A CN201210455766X A CN 201210455766XA CN 201210455766 A CN201210455766 A CN 201210455766A CN 103044328 A CN103044328 A CN 103044328A
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- caprolactamdisulfide
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- rubber vulcanizer
- hexanolactam
- novel rubber
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Abstract
The invention discloses synthesis of novel rubber vulcanizer 1,1'-caprolactamdisulfide. The synthesis of the rubber vulcanizer 1,1'-caprolactamdisulfide is mainly characterized by comprising the following synthesizing steps: dissolving caprolactam in petroleum ether, controlling at a certain temperature, adding S2Cl2 in a dropwise manner, starting reacting and transforming to obtain the novel rubber vulcanizer 1,1'-caprolactamdisulfide, wherein the intermediately generated HCl is combined with the residual caprolactam, and caprolactam hydrochloride is removed through extract of aqueous solution of sodium acetate after the reaction is finished; crude products are separated and are repeatedly suspended under water, the residual petroleum ether is removed through vacuum distillation through the regulation of a pH value; and after the novel rubber vulcanizer 1,1'-caprolactamdisulfide is separated, washed in water and dried to obtain white solid caprolactamdisulfide. Through the synthesis of the novel rubber vulcanizer 1,1'-caprolactamdisulfide disclosed by the invention, the yield is larger than 83%.
Description
Technical field
The invention belongs to rubber synthesis technique field, be mainly synthetic rubber and prepare chemical additive, wear-resistant, anticorrosion with Reinforced Rubber, the characteristic such as corrosion-resistant.Be specially a kind of rubber vulcanization agent 1, the two hexanolactams of 1 '-dithio synthetic.
Background technology
Rubber is used very extensive in modern civilization society, automobile, aircraft, pipeline in the tire of bike and the various chemical industry, joint etc., various electrical equipment in the daily life, all must adopt synthetic rubber, according to different requirements and characteristic, make the rubber item of all size, to satisfy industrial and agricultural production and daily life requisite, but synthetic (perhaps natural rubber) is easily As time goes on, produces aging oxidation, in sweltering heat, can expand and cracking in the arctic weather, the generation of above-mentioned situation will bring great threat to security fields, can cause serious life and property loss, characteristic of the present invention is the specific aim during solving rubber synthesizes, rubber to various different purposes adds the CLD that the present invention produced, can effectively solve ageing of rubber, oxidation, the shortcomings such as aging, for example: in the tire of automobile is made, add the tire that an amount of CLD makes, in advancing at a high speed, no matter heat or cold, tire is easily explosion not, can avoid the generation of security incident.
Summary of the invention
The present invention is intended to develop a kind of novel vulcanizer, is used in the synthetic chloroprene rubber goods, can improve elastomeric physics-chem characteristic, makes it wear-resisting, and the friction of rot-resistant high temperature resistance has great potential use for automotive industry.
Synthesis step is as follows: hexanolactam is dissolved in the sherwood oil, and the control certain temperature drips S2Cl2, begins reaction and transforms and get, and the middle HCl that generates is combined with remaining hexanolactam.Reaction finishes, and hexanolactam hydrochloride (hydrochloride) is removed by the sodium acetate aqueous solution extraction.Crude product is separated and is again suspended in water.Through adjusting pH, remaining sherwood oil is removed by vacuum distilling.Product is separated, washing and the dry finished product that gets.Its principal reaction equation is as follows:
Figure of description
Fig. 1 is production technological process of the present invention.
The below will elaborate by specific embodiment.
[0007] embodiment 1
As shown in Figure 1: in reactor, drop into the hexanolactam that adds 450 kilograms under 1975 kilograms the petroleum ether and stirring behind the nitrogen replacement, be warming up to 40 ° of C and begin to drip 120 kg S2Cl2, add about 3 hours, add rear continuation at stirring reaction under this temperature after 4 hours after the sampling analysis hexanolactam complete reaction, be cooled to room temperature, add 600 kilogram of 20% sodium acetate soln, stir 0.5h, the blowing suction filtration, filter cake put into reactor and add 2700 kilograms water and stir, add again 68 kilograms of 25% liquid caustic soda and adjust pH value.Filtrate is reclaimed solvent, the sherwood oil of remnants in the still kettle, steam and finish, measure the PH value of liquid in the still, rear blowing suction filtration up to standard also adds 350 kilograms of deionized water wash, and product 1 must wet, the two hexanolactams of 1 '-dithio, the product of wetting are carried out drying under reduced pressure, get 215 kilograms of white solids, fusing point 125-130 ° of C(yield 83%).
Claims (3)
1. rubber vulcanization agent 1, synthesizing of the two hexanolactams of 1 '-dithio, be primarily characterized in that synthesis step is as follows: hexanolactam is dissolved in the sherwood oil, and the control certain temperature drips S2Cl2, begin reaction and transform and get, the HCl of middle generation is combined with remaining hexanolactam.Reaction finishes, and hexanolactam hydrochloride (hydrochloride) is removed by the sodium acetate aqueous solution extraction.Crude product is separated and is again suspended in water.Through adjusting pH, remaining sherwood oil is removed by vacuum distilling.Product is separated, washing and the dry finished product that gets.Its principal reaction equation is as follows:
2. described according to claim 1, be primarily characterized in that hexanolactam: S2Cl2: the sherwood oil weight ratio is that 1:0.2-1.5:4-50(is preferred: 1:0.28-0.8:5-10).
3. described according to claim 1 and 2, be primarily characterized in that: drip the temperature-5-100 ° of preferred 10-60 of C(of S2Cl2 ° C).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367496A (en) * | 2015-12-04 | 2016-03-02 | 山东阳谷华泰化工股份有限公司 | Synthetic method of vulcanizing agent 1,1-caprolactam disulfide |
| CN108117517A (en) * | 2018-02-01 | 2018-06-05 | 蔚林新材料科技股份有限公司 | The preparation method of thiofide DTDC |
| CN108658864A (en) * | 2018-04-30 | 2018-10-16 | 杭州布朗生物医药科技有限公司 | A kind of preparation method of 1,1 '-two thiobis caprolactam of vulcanizer |
| CN110143922A (en) * | 2019-06-25 | 2019-08-20 | 山东阳谷华泰化工股份有限公司 | A kind of synthetic method of 1,1 '-dicaprolactam disulfides |
| CN110156691A (en) * | 2019-06-20 | 2019-08-23 | 山东阳谷华泰化工股份有限公司 | A kind of preparation method of curing dicaprolactam |
| CN110256348A (en) * | 2019-06-25 | 2019-09-20 | 山东阳谷华泰化工股份有限公司 | A kind of synthetic method of vulcanizer DTDC |
| CN110683988A (en) * | 2019-09-29 | 2020-01-14 | 山东阳谷华泰化工股份有限公司 | Method for cleanly producing DTDC |
| CN112390756A (en) * | 2020-11-30 | 2021-02-23 | 山东嘉成医药科技有限公司 | Industrial preparation method of N, N' -dithiocaprolactam |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105367496A (en) * | 2015-12-04 | 2016-03-02 | 山东阳谷华泰化工股份有限公司 | Synthetic method of vulcanizing agent 1,1-caprolactam disulfide |
| CN108117517A (en) * | 2018-02-01 | 2018-06-05 | 蔚林新材料科技股份有限公司 | The preparation method of thiofide DTDC |
| CN108658864B (en) * | 2018-04-30 | 2020-11-13 | 杭州布朗生物医药科技有限公司 | Preparation method of rubber vulcanizing agent 1, 1' -dithiobiscaprolactam |
| CN108658864A (en) * | 2018-04-30 | 2018-10-16 | 杭州布朗生物医药科技有限公司 | A kind of preparation method of 1,1 '-two thiobis caprolactam of vulcanizer |
| CN110156691A (en) * | 2019-06-20 | 2019-08-23 | 山东阳谷华泰化工股份有限公司 | A kind of preparation method of curing dicaprolactam |
| CN110156691B (en) * | 2019-06-20 | 2022-03-25 | 山东阳谷华泰化工股份有限公司 | Preparation method of caprolactam disulfide |
| CN110143922A (en) * | 2019-06-25 | 2019-08-20 | 山东阳谷华泰化工股份有限公司 | A kind of synthetic method of 1,1 '-dicaprolactam disulfides |
| CN110256348A (en) * | 2019-06-25 | 2019-09-20 | 山东阳谷华泰化工股份有限公司 | A kind of synthetic method of vulcanizer DTDC |
| CN110143922B (en) * | 2019-06-25 | 2022-06-24 | 山东阳谷华泰化工股份有限公司 | Synthetic method of 1, 1' -dithio-di-caprolactam |
| CN110256348B (en) * | 2019-06-25 | 2022-08-12 | 山东阳谷华泰化工股份有限公司 | Synthetic method of rubber vulcanizing agent DTDC |
| CN110683988A (en) * | 2019-09-29 | 2020-01-14 | 山东阳谷华泰化工股份有限公司 | Method for cleanly producing DTDC |
| CN112390756A (en) * | 2020-11-30 | 2021-02-23 | 山东嘉成医药科技有限公司 | Industrial preparation method of N, N' -dithiocaprolactam |
| CN112390756B (en) * | 2020-11-30 | 2023-07-11 | 山东嘉成医药科技有限公司 | Industrial preparation method of N, N' -dithiocaprolactam |
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Application publication date: 20130417 |