CN102850249A - Preparation method of 1, 1-bis(t-butyl peroxy)-3, 3, 5-trimethylcyclohexane - Google Patents
Preparation method of 1, 1-bis(t-butyl peroxy)-3, 3, 5-trimethylcyclohexane Download PDFInfo
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- CN102850249A CN102850249A CN2012103530871A CN201210353087A CN102850249A CN 102850249 A CN102850249 A CN 102850249A CN 2012103530871 A CN2012103530871 A CN 2012103530871A CN 201210353087 A CN201210353087 A CN 201210353087A CN 102850249 A CN102850249 A CN 102850249A
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Abstract
Belonging to the field of organic peroxide preparation, the invention relates to a preparation method of 1, 1-bis(t-butyl peroxy)-3, 3, 5-trimethylcyclohexane. The method consists of: adding tert-butyl hydroperoxide and 3, 3, 5-trimethylcyclohexanone into a mixing kettle and conducting stirring, separating out a lower aqueous phase; adding sulfuric acid and a recycled mother solution into an acid preparation kettle, and performing stirring; adding a mixed solution of tert-butyl hydroperoxide and 3, 3, 5-trimethylcyclohexanone, and a sulfuric acid solution used for catalysis into a synthesis kettle, and stirring them; introducing a reaction product into a layering trough for layering, mixing a lower aqueous phase sulfuric acid-containing mother solution with sulfuric acid, and introducing an upper 1, 1-bis(t-butyl peroxy)-3, 3, 5-trimethylcyclohexane crude product into a post-treatment kettle; and subjecting the 1, 1-bis(t-butyl peroxy)-3, 3, 5-trimethylcyclohexane crude product in the post-treatment kettle to alkali washing, water scrubbing, drying and filtering, thus obtaining the finished product. The method has the advantages of: environmental protection, raw material saving, and preparation cost reduction.
Description
Technical field
The invention belongs to the preparing technical field of organo-peroxide, be specifically related to a kind of 1,1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane.
Background technology
1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane also claims 1,1-di-tert-butyl peroxide-3,3,5-trimethyl-cyclohexane (being called for short initiator CH335), English name is: 1,1-Bis (t-butyl peroxy)-3,3,5-Tri Methyl Cyclo Hexane(is called for short TMCH).Its molecular formula is: C
17H
34O
4Molecular weight is: 302.5; Structural formula is:
TMCH is a kind of ketal class organo-peroxide commonly used, mainly is used as the initiators for polymerization of vinylbenzene and comonomer thereof etc., polyvinyl chloride, polyethylene, polystyrene and unsaturated polyester cross-linking agent, and silicon rubber vulcanization agent.
Take sulfuric acid or other acid as catalyzer, take tertbutyl peroxide as oxidizer catalytic oxidation 3,3, it is method the most frequently used in the suitability for industrialized production that the 5-trimethylcyclohexanone prepares TMCH, the method is commonly referred to the acid catalysis synthesis method, and existing bibliographical information, such as US Patent No. 4052464, China Patent Publication No. CN102336694A ［ synthetic method of bis(t-butylperoxy) ketal ］ and CN102336695A ［ production method of bis(t-butylperoxy) ketal ］.
Although under existing acid catalysis synthesis method, it is quotidian that the aqueous phase of reaction system contains a large amount of sulfuric acid, especially in actual production, find, if this water is back to reaction system, the rising of the trimethyl carbinol in the product, di-t-butyl peroxide component and other by-products content that tends to induce reaction, thus have a strong impact on quality and the yield of product, and therefore generally believing in industrial production does not have reuse to be worth, Chang Zuowei discharging of waste liquid, the utmost point do not meet green production and environmental friendliness.Yet if from the angle of protection of the environment it is processed, the high acid-bearing wastewater treatment process of the so this organo-peroxide that contains difficult degradation comparatively complexity and cost is high.
" initiator CH335 wastewater treatment and the process for reclaiming " that Chinese invention patent Granted publication CN102173522A recommends, it is to collect from the production equipment sewage draining exit to produce spent acid, in every liter of spent acid, add the 1-2g S-WAT, at the 50-60 ℃ of lower 90-120min that stirs, again underpressure distillation, the distillate condensation and be cooled to room temperature after layering, reclaim the organic phase on upper strata, lower floor's aqueous-phase reflux, until distillate is during at normal temperatures without layering, adopt air distillation to obtain low concentration wastewater and be neutralized to pH7-8, finally by hydrolysis-catalytic oxidation and after the little electrolysis process of C-Fe is processed qualified discharge, and the concentrating waste acid after distilling reclaims the vitriol oil through underpressure distillation.Although this treatment process can embody the strong point of its specification sheets 0019-0023 section, objectively there are following 2 shortcoming: the one, only realized the part utilization of resource, because still have a large amount of waste water and dangerous solid waste; The 2nd, complex treatment process and energy consumption are high, cause processing cost large.Therefore this patent scheme does not fundamentally solve comprehensive utilization and cleaner production problem.To this, the applicant has carried out long-term exploration and practice repeatedly, finds a way to resolve the problem, and technical scheme described below produces under this background.
Summary of the invention
Task of the present invention is to provide a kind of and can avoids vitriolated mother liquor to use as discharging of waste liquid economizing in raw materials, protection of the environment and reduce 1 of preparation cost, 1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane.
Task of the present invention is finished like this, and is a kind of 1,1-bis(t-butylperoxy)-3,3, and the preparation method of 5-trimethyl-cyclohexane may further comprise the steps:
A) tertbutyl peroxide and 3,3,5-trimethylcyclohexanone are joined in the mixing kettle, mix under the temperature control condition, leave standstill this and tell lower floor's water simultaneously, obtain the mixed solution of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) sulfuric acid and reuse mother liquor are joined in the complex acid still, mix under the temperature control condition, obtain the sulphuric acid soln that catalysis is used;
C) with the mixed solution of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction, obtains reaction product;
D) reaction product is introduced the layering of layering groove, obtain upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product and the vitriolated mother liquor of lower floor's water, and the vitriolated mother liquor of lower floor's water led get back to step B) in mix with sulfuric acid, and with upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product import in the aftertreatment still;
E) with 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product through alkali cleaning, washing, drying with after filtering, get 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane finished product successively.
In a specific embodiment of the present invention, the mass percent concentration of the tertbutyl peroxide steps A) is 68～85%, described 3,3, the 5-trimethylcyclohexanone is that mass percent concentration is 99% technical pure, the mol ratio of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone is 2.05～3.00 ︰ 1.
In another specific embodiment of the present invention, steps A) temperature control described in is that temperature is controlled to be 5～30 ℃, the described rotating speed that mixes is 50～150r/min, and the described time that mixes is 〉=10min that the described time of leaving standstill is 〉=15min.
In another specific embodiment of the present invention, step B) sulfuric acid described in is that mass percent concentration is 98% technical pure, the sulphuric acid soln mass percent concentration that described catalysis is used is 60～70%, described sulfuric acid and steps A) described in 3, the mol ratio of 3,5-trimethylcyclohexanone is 1.010～2.164 ︰ 1.
In another specific embodiment of the present invention, step B) temperature control described in is that temperature is controlled to be 5～30 ℃, and the described rotating speed that mixes is 50～150r/min, and the described time that mixes is 〉=10min.
Also have in the specific embodiment step C of the present invention) described in the control temperature of reaction be that temperature of reaction is controlled to be 5～30 ℃, the rotating speed of described stirring reaction is 50～150r/min, the described reaction times is 2.5～5.0h.
Technical scheme provided by the present invention since the vitriolated mother liquor of lower floor's water led get back to step B) in mixes with sulfuric acid, sustainable participation reacts, and has both avoided discharging of waste liquid and is conducive to protection of the environment, has saved raw material again and is conducive to reduce preparation cost.
Description of drawings
Accompanying drawing is preparation method's of the present invention process flow sheet.
Embodiment
Embodiment 1:
The step that comprises by technical process shown in Figure 1 is as follows:
A) with 613.9Kg tertbutyl peroxide (mass percent concentration is 85%) and 400Kg 3,3,5-trimethylcyclohexanone (mass percent concentration is 99%) joins in the mixing kettle, temperature control is below 5 ℃, and mixing speed mixes 10min under the 120r/min condition, leave standstill 60min after, tell the water 39.91Kg of lower floor, obtain the mixed solution 974.09Kg of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) 114.78Kg sulfuric acid (mass percent concentration is 98%) and 885.22Kg reuse mother liquor (the sulfur acid mass percent concentration is 55.1%) are joined in the complex acid still, temperature control is below 5 ℃, mixing speed mixes 30min under the 120r/min condition, obtain the sulphuric acid soln 1000Kg that catalysis is used;
C) with the mixed solution of 974.09Kg tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that 1000Kg catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction is below 5 ℃, and mixing speed reacts 5h under the 120r/min condition, obtain reaction product;
D) reaction product is introduced left standstill the 1h layering in the layering groove, obtain 1,1-bis(t-butylperoxy)-3, the vitriolated mother liquor 1089.46Kg of 3,5-trimethyl-cyclohexane crude product and lower floor's water, and the vitriolated mother liquor 885.22Kg of lower floor's water led get back to step B) mixes with sulfuric acid in, upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product 882.1Kg import in the aftertreatment still;
E) 882.1Kg 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product gets 1,1-bis(t-butylperoxy)-3,3 after conventional alkali cleaning, washing, drying, filtration, 5-trimethyl-cyclohexane finished product 858.2Kg.Detect through GC, 1,1-bis(t-butylperoxy)-3,3, the content of 5-trimethyl-cyclohexane are 96.3%, and yield is 96.7%.
Embodiment 2:
A) with 700Kg tertbutyl peroxide (mass percent concentration is 80%) and 400Kg 3,3,5-trimethylcyclohexanone (mass percent concentration is 99%) joins in the mixing kettle, temperature control is below 10 ℃, and mixing speed mixes 20min under the 80r/min condition, leave standstill 50min after, tell the water 42.7Kg of lower floor, obtain the mixed solution 1057.3Kg of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) 205.08Kg sulfuric acid (mass percent concentration is 98%) and 654.92Kg reuse mother liquor (the sulfur acid mass percent concentration is 50.7%) are joined in the complex acid still, temperature control is below 10 ℃, mixing speed mixes 20min under the 80r/min condition, obtain the sulphuric acid soln 860Kg that catalysis is used;
C) with the mixed solution of 1057.3Kg tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that 860Kg catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction is below 10 ℃, and mixing speed reacts 4.5h under the 80r/min condition, obtain reaction product;
D) reaction product is introduced left standstill the 1h layering in the layering groove, obtain 1,1-bis(t-butylperoxy)-3, the vitriolated mother liquor 1051.12Kg of 3,5-trimethyl-cyclohexane crude product and lower floor's water, and the vitriolated mother liquor 654.92Kg of lower floor's water led get back to step B) mixes with sulfuric acid in, upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product 863.75Kg import in the aftertreatment still;
E) 863.75Kg 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product gets 1,1-bis(t-butylperoxy)-3 after conventional alkali cleaning, washing, drying, filtration, 3,5-trimethyl-cyclohexane finished product 841.47Kg.Detect through GC, 1,1-bis(t-butylperoxy)-3,3, the content of 5-trimethyl-cyclohexane are 97.4%, and yield is 95.9%.
Embodiment 3:
A) with 814.6Kg tertbutyl peroxide (mass percent concentration is 75%) and 400Kg 3,3,5-trimethylcyclohexanone (mass percent concentration is 99%) joins in the mixing kettle, temperature control is below 15 ℃, and mixing speed mixes 30min under the 50r/min condition, leave standstill 40min after, tell the water 45.62Kg of lower floor, obtain the mixed solution 1169.01Kg of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) 255.96Kg sulfuric acid (mass percent concentration is 98%) and 474.04Kg reuse mother liquor (the sulfur acid mass percent concentration is 45.6%) are joined in the complex acid still, temperature control is below 15 ℃, mixing speed mixes 10min under the 50r/min condition, obtain the sulphuric acid soln 730Kg that catalysis is used;
C) with the mixed solution of 1169.01Kg tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that 730Kg catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction is below 15 ℃, and mixing speed reacts 4h under the 50r/min condition, obtain reaction product;
D) reaction product is introduced left standstill the 1h layering in the layering groove, obtain 1,1-bis(t-butylperoxy)-3, the vitriolated mother liquor 1023.63Kg of 3,5-trimethyl-cyclohexane crude product and lower floor's water, and the vitriolated mother liquor 474.04Kg of lower floor's water led get back to step B) mixes with sulfuric acid in, upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product 872.88Kg import in the aftertreatment still;
E) 872.88Kg 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product gets 1,1-bis(t-butylperoxy)-3 after conventional alkali cleaning, washing, drying, filtration, 3,5-trimethyl-cyclohexane finished product 849.34Kg.Detect through GC, 1,1-bis(t-butylperoxy)-3,3, the content of 5-trimethyl-cyclohexane are 96.8%, and yield is 96.2%.
Embodiment 4:
A) with 919.28Kg tertbutyl peroxide (mass percent concentration is 72%) and 400Kg 3,3,5-trimethylcyclohexanone (mass percent concentration is 99%) joins in the mixing kettle, temperature control is below 20 ℃, and mixing speed mixes 30min under the 60r/min condition, leave standstill 30min after, tell the water 47.8Kg of lower floor, obtain the mixed solution 1271.48Kg of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) 272.29Kg sulfuric acid (mass percent concentration is 98%) and 337.71Kg reuse mother liquor (the sulfur acid mass percent concentration is 40.2%) are joined in the complex acid still, temperature control is below 20 ℃, mixing speed mixes 30min under the 60r/min condition, obtain the sulphuric acid soln 610Kg that catalysis is used;
C) with the mixed solution of 1271.48Kg tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that 610Kg catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction is below 20 ℃, and mixing speed reacts 3.5h under the 60r/min condition, obtain reaction product;
D) reaction product is introduced left standstill the 1h layering in the layering groove, obtain 1,1-bis(t-butylperoxy)-3, the vitriolated mother liquor 1001.52Kg of 3,5-trimethyl-cyclohexane crude product and lower floor's water, and the vitriolated mother liquor 337.71Kg of lower floor's water led get back to step B) mixes with sulfuric acid in, upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product 877.47Kg import in the aftertreatment still;
E) 877.47Kg 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product gets 1,1-bis(t-butylperoxy)-3 after conventional alkali cleaning, washing, drying, filtration, 3,5-trimethyl-cyclohexane finished product 854.64Kg.Detect through GC, 1,1-bis(t-butylperoxy)-3,3, the content of 5-trimethyl-cyclohexane are 96.5%, and yield is 96.5%.
Embodiment 5:
A) with 1018.28Kg tertbutyl peroxide (mass percent concentration is 70%) and 400Kg 3,3,5-trimethylcyclohexanone (mass percent concentration is 99%) joins in the mixing kettle, temperature control is below 25 ℃, and mixing speed mixes 20min under the 100r/min condition, leave standstill 20min after, tell the water 49.9Kg of lower floor, obtain the mixed solution 1368.39Kg of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) 265.67Kg sulfuric acid (mass percent concentration is 98%) and 234.33Kg reuse mother liquor (the sulfur acid mass percent concentration is 34.0%) are joined in the complex acid still, temperature control is below 25 ℃, mixing speed mixes 20min under the 100r/min condition, obtain the sulphuric acid soln 500Kg that catalysis is used;
C) with the mixed solution of 1368.39Kg tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that 500Kg catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction is below 25 ℃, and mixing speed reacts 3h under the 100r/min condition, obtain reaction product;
D) reaction product is introduced left standstill the 1h layering in the layering groove, obtain 1,1-bis(t-butylperoxy)-3, the vitriolated mother liquor 1000.33Kg of 3,5-trimethyl-cyclohexane crude product and lower floor's water, and the vitriolated mother liquor 234.33Kg of lower floor's water led get back to step B) mixes with sulfuric acid in, upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product 865.56Kg import in the aftertreatment still;
E) 865.56Kg 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product gets 1,1-bis(t-butylperoxy)-3 after conventional alkali cleaning, washing, drying, filtration, 3,5-trimethyl-cyclohexane finished product 844.08Kg.Detect through GC, 1,1-bis(t-butylperoxy)-3,3, the content of 5-trimethyl-cyclohexane are 97.2%, and yield is 96.0%.
Embodiment 6:
A) with 1123.1Kg tertbutyl peroxide (mass percent concentration is 68%) and 400Kg 3,3,5-trimethylcyclohexanone (mass percent concentration is 99%) joins in the mixing kettle, temperature control is below 30 ℃, and mixing speed mixes 10min under the 150r/min condition, leave standstill 15min after, tell the water 50.54Kg of lower floor, obtain the mixed solution 1472.57Kg of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) 239.76Kg sulfuric acid (mass percent concentration is 98%) and 160.24Kg reuse mother liquor (the sulfur acid mass percent concentration is 28.1%) are joined in the complex acid still, temperature control is below 3 ℃, mixing speed mixes 10min under the 150r/min condition, obtain the sulphuric acid soln 400Kg that catalysis is used;
C) with the mixed solution of 1472.57Kg tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that 400Kg catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction is below 3 ℃, and mixing speed reacts 2.5h under the 150r/min condition, obtain reaction product;
D) reaction product is introduced left standstill the 1h layering in the layering groove, obtain 1,1-bis(t-butylperoxy)-3, the vitriolated mother liquor 996.26Kg of 3,5-trimethyl-cyclohexane crude product and lower floor's water, and the vitriolated mother liquor 160.24Kg of lower floor's water led get back to step B) mixes with sulfuric acid in, upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product 873.81Kg import in the aftertreatment still;
E) 873.81Kg 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product gets 1,1-bis(t-butylperoxy)-3 after conventional alkali cleaning, washing, drying, filtration, 3,5-trimethyl-cyclohexane finished product 850.22Kg.Detect through GC, 1,1-bis(t-butylperoxy)-3,3, the content of 5-trimethyl-cyclohexane are 96.7%, and yield is 96.2%.
Claims (6)
1.
A kind of 1,1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane is characterized in that may further comprise the steps:
A) tertbutyl peroxide and 3,3,5-trimethylcyclohexanone are joined in the mixing kettle, mix under the temperature control condition, leave standstill this and tell lower floor's water simultaneously, obtain the mixed solution of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone;
B) sulfuric acid and reuse mother liquor are joined in the complex acid still, mix under the temperature control condition, obtain the sulphuric acid soln that catalysis is used;
C) with the mixed solution of tertbutyl peroxide and 3,3,5-trimethylcyclohexanone, and the sulphuric acid soln that catalysis is used joins stirring reaction in the synthesis reactor, and the control temperature of reaction, obtains reaction product;
D) reaction product is introduced the layering of layering groove, obtain upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product and the vitriolated mother liquor of lower floor's water, and the vitriolated mother liquor of lower floor's water led get back to step B) in mix with sulfuric acid, and with upper strata 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product import in the aftertreatment still;
E) with 1 in the aftertreatment still, 1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane crude product through alkali cleaning, washing, drying with after filtering, get 1,1-bis(t-butylperoxy)-3,3,5-trimethyl-cyclohexane finished product successively.
2.
According to claim 11,1-bis(t-butylperoxy)-3, the preparation method of 3,5-trimethyl-cyclohexane is characterized in that steps A) described in the mass percent concentration of tertbutyl peroxide be 68～85%, described 3,3,5-trimethylcyclohexanone is that mass percent concentration is 99% technical pure, tertbutyl peroxide and 3, the mol ratio of 3,5-trimethylcyclohexanone is 2.05～3.00 ︰ 1.
3.
According to claim 11,1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane, it is characterized in that steps A) described in temperature control be that temperature is controlled to be 5～30 ℃, the described rotating speed that mixes is 50～150r/min, and the described time that mixes is 〉=10min that the described time of leaving standstill is 〉=15min.
4.
According to claim 11,1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane, it is characterized in that step B) described in sulfuric acid be that mass percent concentration is 98% technical pure, the sulphuric acid soln mass percent concentration that described catalysis is used is 60～70%, described sulfuric acid and steps A) described in 3, the mol ratio of 3,5-trimethylcyclohexanone is 1.010～2.164 ︰ 1.
5.
According to claim 11,1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane, it is characterized in that step B) described in temperature control be that temperature is controlled to be 5～30 ℃, the described rotating speed that mixes is 50～150r/min, and the described time that mixes is 〉=10min.
6.
According to claim 11,1-bis(t-butylperoxy)-3,3, the preparation method of 5-trimethyl-cyclohexane, it is characterized in that step C) described in the control temperature of reaction be that temperature of reaction is controlled to be 5～30 ℃, the rotating speed of described stirring reaction is 50～150r/min, and the described reaction times is 2.5～5.0h
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| CN103360623A (en) * | 2013-07-07 | 2013-10-23 | 天长市天广有机玻璃有限公司 | Preparation method of peroxide poly-hybrid ketal solution |
| CN103421209A (en) * | 2013-07-07 | 2013-12-04 | 天长市天广有机玻璃有限公司 | Medium temperature curing initiator suitable for unsaturated resin products |
| CN108373435A (en) * | 2018-04-28 | 2018-08-07 | 江苏强盛功能化学股份有限公司 | A kind of 1,1- is bis-（T-butylperoxy）The recoverying and utilizing method of -3,3,5- trimethyl-cyclohexane soda-wash waters |
| CN113387859A (en) * | 2021-06-18 | 2021-09-14 | 常熟市滨江化工有限公司 | Recycling treatment method of 1, 1-bis (tert-butyl peroxy) -3,3, 5-trimethylcyclohexane waste material |
| CN113880743A (en) * | 2021-11-16 | 2022-01-04 | 山东阳谷华泰化工股份有限公司 | Preparation method of 1, 1-bis (tert-butyl peroxy) -3,3,5 trimethylcyclohexane |
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| CN103360623A (en) * | 2013-07-07 | 2013-10-23 | 天长市天广有机玻璃有限公司 | Preparation method of peroxide poly-hybrid ketal solution |
| CN103421209A (en) * | 2013-07-07 | 2013-12-04 | 天长市天广有机玻璃有限公司 | Medium temperature curing initiator suitable for unsaturated resin products |
| CN103421209B (en) * | 2013-07-07 | 2015-03-25 | 天长市天广有机玻璃有限公司 | Medium temperature curing initiator suitable for unsaturated resin products |
| CN108373435A (en) * | 2018-04-28 | 2018-08-07 | 江苏强盛功能化学股份有限公司 | A kind of 1,1- is bis-（T-butylperoxy）The recoverying and utilizing method of -3,3,5- trimethyl-cyclohexane soda-wash waters |
| CN113387859A (en) * | 2021-06-18 | 2021-09-14 | 常熟市滨江化工有限公司 | Recycling treatment method of 1, 1-bis (tert-butyl peroxy) -3,3, 5-trimethylcyclohexane waste material |
| CN113387859B (en) * | 2021-06-18 | 2022-04-26 | 常熟市滨江化工有限公司 | Recycling treatment method of 1, 1-bis (tert-butyl peroxy) -3,3, 5-trimethylcyclohexane waste material |
| CN113880743A (en) * | 2021-11-16 | 2022-01-04 | 山东阳谷华泰化工股份有限公司 | Preparation method of 1, 1-bis (tert-butyl peroxy) -3,3,5 trimethylcyclohexane |
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