CN103508976A

CN103508976A - Method for producing rubber vulcanization accelerator NS

Info

Publication number: CN103508976A
Application number: CN201310466202.0A
Authority: CN
Inventors: 朱军
Original assignee: Kemai Chemical Co Ltd
Current assignee: Kemai Chemical Co Ltd
Priority date: 2013-09-30
Filing date: 2013-09-30
Publication date: 2014-01-15

Abstract

The invention discloses a method for producing a rubber vulcanization accelerator NS (N-tert-butyl-benzothiazole sulfonamide), which comprises the following steps: adding mixed solution with a volume ratio of methanol to tert-butylamine of (0.6 to 0.8):1 into an oxidation pot and under the conditions of a temperature of 30 to 60 DEG C and a rotating speed of 800 revolutions per minute, adding slurry with a mass ratio of an accelerator M to methanol of 1:1 at a flow rate of 2 ml per minute; simultaneously, dropwise adding hydrogen peroxide solution with mass content of 8 to 12 percent into the solution at the flow rate of 2 ml per minute, stopping dropwise adding the hydrogen peroxide after 90 minutes, carrying out heat preservation for 10 minutes and starting to distill to recover methanol; carrying out suction filtration, washing, filtration and drying on the obtained product to obtain the rubber vulcanization accelerator NS product. The method has a simple process and utilizes methanol to replace water so as to reduce produced wastewater by over 80 percent relative to a conventional process; moreover, the wastewater does not contain salt, so that cost of wastewater treatment is greatly reduced. The process is easy for industrialization, a small quantity of tert-butylamine is used and the yield of the accelerator NS is over 99 percent.

Description

Produce the method for rubber vulcanization accelerator NS

Technical field

The production method that the present invention relates to a kind of rubber vulcanization accelerator N-tertiary butyl-2-[4-morpholinodithio sulphenamide (NS), belongs to rubber vulcanization accelerator NS production technical field.

Background technology

Along with the development of rubber industry, the research of vulcanization accelerator is more and more subject to people's attention with production.Vulcanization accelerator plays very important effect in Vulcanization Process of Rubber, it can accelerate reacting of rubber and vulcanizing agent greatly, boost productivity, also can improve the physical and mechanical properties of vulcanized rubber, NS is the requisite a kind of primary accelerator of current rubber industry simultaneously.That accelerator NS has is anti-scorch, safe, nontoxic, vulcanize the functions such as fast.Document (Guangdong chemical industry, 2006,5:16) reported the method that oxidation style is synthesized NS.Captax, TERTIARY BUTYL AMINE, dilute sulphuric acid, water etc. are added in reactor and stirred, make its salify; With hydrogen peroxide, as oxygenant, react cooling, suction filtration, washing, filtration, the dry product that to obtain.The TERTIARY BUTYL AMINE amount that this method is used is large, and the yield of accelerator NS is not high.Document (chemical science and technology market, 2001,4:24) reported the production method of new type NS.Captax, TERTIARY BUTYL AMINE, dilute sulphuric acid, water etc. are added in reactor and stirred, make its salify; With clorox, as oxygenant, react cooling, suction filtration, washing, filtration, the dry product that to obtain.This method accelerator NS yield is low, and produces a large amount of brine wastes, is difficult for processing.

Summary of the invention

The invention discloses a kind of take methyl alcohol as solvent, hydrogen peroxide be two methods of oxygenant, produce the method for rubber vulcanization accelerator NS, the method is simple to operate, TERTIARY BUTYL AMINE consumption is little, good product quality, yield are high, it is characterized in that comprising following process:

The mixed solution that is 0.6～0.8:1 by the volume ratio of methyl alcohol and TERTIARY BUTYL AMINE joins in stills for air blowing, at 30-60 ℃, rotating speed, be under the condition of 800 revs/min, flow velocity with 2ml/ minute, add mass ratio 1:1 captax: the slip of methyl alcohol with the flow velocity of 2ml/ minute, drips the hydrogen peroxide solution that mass content is 8-12% simultaneously in solution, after 90 minutes, stop dripping hydrogen peroxide, be incubated 10 minutes, start Distillation recovery methyl alcohol; Product is through suction filtration, washing, filtration, the dry rubber accelerator NS product that to obtain, and the yield of accelerator NS reaches more than 99%.

The invention has the advantages that: the method process is simple, with methyl alcohol, replaces water, the older technique of waste water of producing is reduced more than 80%, and do not contain salinity in waste water, greatly reduce the cost of wastewater treatment.This technique is easy to industrialization, and the TERTIARY BUTYL AMINE of use is few, and the yield of accelerator NS reaches more than 99%.

Embodiment

Embodiment 1:

The mixed solution that is 0.6:1 by the volume ratio of methyl alcohol and TERTIARY BUTYL AMINE joins in stills for air blowing, at 30 ℃, rotating speed, be under the condition of 800 revs/min, flow velocity with 2ml/ minute, add mass ratio 1:1 captax: the slip of methyl alcohol, simultaneously with the flow velocity of 2ml/ minute, is 12% hydrogen peroxide solution to dripping mass content in solution, after 90 minutes, stop dripping hydrogen peroxide, be incubated 10 minutes, start Distillation recovery methyl alcohol; Product is through suction filtration, washing, filtration, the dry rubber accelerator NS product that to obtain, and the yield of accelerator NS reaches more than 99%.

Embodiment 2:

The mixed solution that is 0.7:1 by the volume ratio of methyl alcohol and TERTIARY BUTYL AMINE joins in stills for air blowing, at 45 ℃, rotating speed, be under the condition of 800 revs/min, flow velocity with 2ml/ minute, add mass ratio 1:1 captax: the slip of methyl alcohol, simultaneously with the flow velocity of 2ml/ minute, is 10% hydrogen peroxide solution to dripping mass content in solution, after 90 minutes, stop dripping hydrogen peroxide, be incubated 10 minutes, start Distillation recovery methyl alcohol; Product is through suction filtration, washing, filtration, the dry rubber accelerator NS product that to obtain, and the yield of accelerator NS reaches more than 99%.

Embodiment 3:

The mixed solution that is 0.8:1 by the volume ratio of methyl alcohol and TERTIARY BUTYL AMINE joins in stills for air blowing, at 60 ℃, rotating speed, be under the condition of 800 revs/min, flow velocity with 2ml/ minute, add mass ratio 1:1 captax: the slip of methyl alcohol, simultaneously with the flow velocity of 2ml/ minute, is 8% hydrogen peroxide solution to dripping mass content in solution, after 90 minutes, stop dripping hydrogen peroxide, be incubated 10 minutes, start Distillation recovery methyl alcohol; Product is through suction filtration, washing, filtration, the dry rubber accelerator NS product that to obtain, and the yield of accelerator NS reaches more than 99%.

Claims

1. a method of producing rubber vulcanization accelerator NS, it is characterized in that: the mixed solution that is 0.6～0.8:1 by the volume ratio of methyl alcohol and TERTIARY BUTYL AMINE joins in stills for air blowing, at 30-60 ℃, rotating speed, be under the condition of 800 revs/min, with the flow velocity of 2ml/ minute, add mass ratio 1:1 captax: the slip of methyl alcohol; With the flow velocity of 2ml/ minute, in solution, drip the hydrogen peroxide solution that mass content is 8-12% simultaneously, after 90 minutes, stop dripping hydrogen peroxide, be incubated 10 minutes, start Distillation recovery methyl alcohol; Product is through suction filtration, washing, filtration, the dry rubber accelerator NS product that to obtain.