CN103539759A - Method for reducing water used in synthesis process of accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) - Google Patents
Method for reducing water used in synthesis process of accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) Download PDFInfo
- Publication number
- CN103539759A CN103539759A CN201310485068.9A CN201310485068A CN103539759A CN 103539759 A CN103539759 A CN 103539759A CN 201310485068 A CN201310485068 A CN 201310485068A CN 103539759 A CN103539759 A CN 103539759A
- Authority
- CN
- China
- Prior art keywords
- mbt
- water
- reaction
- water used
- tert
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D277/70—Sulfur atoms
- C07D277/76—Sulfur atoms attached to a second hetero atom
- C07D277/80—Sulfur atoms attached to a second hetero atom to a nitrogen atom
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for reducing water used in the production process of a rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide). The method comprises the following processes: adding water and a raw material MBT (2-mercaptobenzothiazole) to a stirring kettle in proportion and starting stirring; adding anionic or non-ionic surfactants accounting for 0.5-2% of the dry material MBT by mass to the stirring kettle and continuing stirring to improve the wettability of MBT; conveying MBT slurry to a reaction kettle to undergo reaction, wherein the reaction conditions are not changed. The method has the advantages that after adding the surfactants, the wettability of MBT is changed, the surface energy of the material is reduced, the material can be mixed with water uniformly, the fluidity becomes good and the water used for beating can be reduced by 40% at most; meanwhile, the material dispersibility can be enhanced in the reaction process, reaction is carried out smoothly and the product yield is improved by 1%.
Description
Technical field
The present invention relates to a kind of method of economizing on water in a kind of sulfenamide rubber vulcanization accelerator N-tertiary butyl-2-[4-morpholinodithio sulphenamide (TBBS) production process, belong to sulfenamide thiofide 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.Accelerator TBBS (N tert butyl benzothiazole 2 sulfenamide) becomes " standard promotor " because of its excellent property.Because it does not exist the carcinogenic problem of nitrosamine, as the novel sulfenamide class promotor of environment-friendly high-efficiency, there is good development prospect, TBBS has now become one of promotor kind leading on domestic and international market.In TBBS is synthetic, 2-mercaptobenzothiazole (MBT) laggardly enters reactor and participates in reaction through pulling an oar as raw material.But because MBT wetting ability is poor, pulping process is very difficult, and material swims in surface, mix inhomogeneously with water, impact is carried, and therefore virtually needs to strengthen making beating water consumption to guarantee M slurry evenly, and good fluidity, is easy to control simultaneously.Yet along with the increasing of environmental protection pressure, the wastewater problem in auxiliary agent production process also becomes a difficult problem urgently to be resolved hurrily.The wastewater flow rate how reducing in production process is a difficult problem of pendulum in face of producers.
Summary of the invention
The object of the present invention is to provide a kind of method that reduces water in rubber vulcanizing accelerator TBBS production process, for achieving the above object, the present invention is realized by following technical proposals:
Reduce a method for water in rubber vulcanizing accelerator TBBS production process, comprise following process:
1. by MBT, than for 1:2～3, in stirring tank, add water and raw material MBT with quality, open and stir;
2. to the negatively charged ion or the nonionogenic tenside that add the 0.5%-2% of MBT siccative quality in stirring tank, continue to stir 5-10min;
3. MBT slurry is delivered to TBBS oxidizing reactor and carries out oxidizing reaction.
The preferred sapn of negatively charged ion or nonionogenic tenside, the condenses op series of alizarin assistant and alkylphenol and oxyethane.
The same original production process of oxidation reaction condition.
The invention has the advantages that: add the wetting property that has changed MBT after tensio-active agent, reduced material surface can, can mix with water, mobility improves, making beating water can reduce by 40% at most.In reaction process, can strengthen material dispersiveness, be beneficial to reaction and carry out smoothly, product yield improves 1% simultaneously.
Embodiment
Embodiment 1:
By 800kg water and 300kgMBT, insert in stirring tank and pull an oar.Do not add tensio-active agent.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 91.5%.
Embodiment 2:
By 800kg water and 300kgMBT, insert in stirring tank and pull an oar.The condenses op-10 that adds tensio-active agent alkylphenol and oxyethane is 3kg, continues to stir 6min.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 92.5%.
Embodiment 3:
By 600kg water and 300kgMBT, insert in stirring tank and pull an oar.Do not add tensio-active agent.Making beating difficulty, MBT mixes inhomogeneous with water, and slip is difficult to carry.
Embodiment 4:
By 600kg water and 300kgMBT, insert in stirring tank and pull an oar.The condenses op-10 that adds tensio-active agent alkylphenol and oxyethane is 6kg, continues to stir 10min.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 92.4%.
Embodiment 5:
By 900kg water and 300kgMBT, insert in stirring tank and pull an oar.The condenses op-10 that adds tensio-active agent alkylphenol and oxyethane is 6kg, continues to stir 8min.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 93%.
Embodiment 6:
By 900kg water and 300kgMBT, insert in stirring tank and pull an oar.Add tensio-active agent alizarin assistant 6kg, continue to stir 7min.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 93%.
Embodiment 7:
By 900kg water and 300kgMBT, insert in stirring tank and pull an oar.Add tensio-active agent sodium alkyl benzene sulfonate 5kg, continue to stir 8min.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 92.5%.
Embodiment 8:
By 900kg water and 300kgMBT, insert in stirring tank and pull an oar.Add tensio-active agent peregal 4kg, continue to stir 10min.After mixing, M slurry is beaten to reactor and TERTIARY BUTYL AMINE and participated in reacting, react end and filter, be dried, weigh, product yield 92.7%.
Although above the preferred embodiments of the present invention are described; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing from the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, within these all belong to protection scope of the present invention.
Claims (2)
1. reduce a method for water in rubber vulcanizing accelerator TBBS production process, it is characterized in that comprising following process:
1) by MBT, than for 1:2～3, in stirring tank, add water and raw material MBT with quality, open and stir;
2), to the negatively charged ion or the nonionogenic tenside that add the 0.5%-2% of MBT siccative quality in stirring tank, continue to stir 5-10min;
3) MBT slurry is delivered to TBBS oxidizing reactor and carries out oxidizing reaction.
2. the method for claim 1, is characterized in that described ionic surface active agent is sapn, the condenses op series of alizarin assistant and alkylphenol and oxyethane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310485068.9A CN103539759A (en) | 2013-10-16 | 2013-10-16 | Method for reducing water used in synthesis process of accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310485068.9A CN103539759A (en) | 2013-10-16 | 2013-10-16 | Method for reducing water used in synthesis process of accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103539759A true CN103539759A (en) | 2014-01-29 |
Family
ID=49963665
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310485068.9A Pending CN103539759A (en) | 2013-10-16 | 2013-10-16 | Method for reducing water used in synthesis process of accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103539759A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0180869A2 (en) * | 1984-11-08 | 1986-05-14 | Bayer Ag | Process for the preparation of storage-stable benzothiazole-sulfenamides |
| CN101407344A (en) * | 2008-11-12 | 2009-04-15 | 山东阳谷华泰化工有限公司 | Process for treating waste water of rubber vulcanization accelerator NS production |
| CN102285939A (en) * | 2011-08-25 | 2011-12-21 | 科迈化工股份有限公司 | Method for preparing accelerator TBBS (N-tert-butylbenzothiazole-2-sulphenamide) |
-
2013
- 2013-10-16 CN CN201310485068.9A patent/CN103539759A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0180869A2 (en) * | 1984-11-08 | 1986-05-14 | Bayer Ag | Process for the preparation of storage-stable benzothiazole-sulfenamides |
| CN101407344A (en) * | 2008-11-12 | 2009-04-15 | 山东阳谷华泰化工有限公司 | Process for treating waste water of rubber vulcanization accelerator NS production |
| CN102285939A (en) * | 2011-08-25 | 2011-12-21 | 科迈化工股份有限公司 | Method for preparing accelerator TBBS (N-tert-butylbenzothiazole-2-sulphenamide) |
Non-Patent Citations (3)
| Title |
|---|
| 徐万平等: "硫化促进剂NS的合成研究", 《精细化工》 * |
| 樊云峰: "硫化促进剂NS的现状和发展动态", 《江苏化工》 * |
| 蔡玉照: "硫化促进剂NS的新型合成工艺研究", 《山东化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101704687B (en) | Method for producing potassium sulphate by decomposing potassium feldspar at low temperature | |
| CN102424394B (en) | Process for preparing water glass from silicon micropowder by using wet method | |
| CN108017299B (en) | Grinding aid and application thereof | |
| CN103332700B (en) | Method for preparing potassium borofluoride through fluorine-containing wastewater | |
| CN108017300B (en) | Cement grinding method and cement grinding aid | |
| CN103979584B (en) | A kind of boric sludge is for Magnesium Carbonate Light 41-45 technique | |
| CN103274632B (en) | Enhanced cement grinding aid and preparation method thereof | |
| CN101993085B (en) | Method for producing white carbon black for toothpaste from fly ash | |
| CN103359699B (en) | Wet-process phosphoric acid dissolving technology | |
| CN105524014A (en) | Purification method of rubber vulcanization accelerator 2-mercaptobenzothiazole | |
| CN102431976B (en) | Method for recovering sulfur and iron resources through reducing and decomposing titanium white waste slag green vitriol by sulfur | |
| CN104478276A (en) | Granulated blast furnace slag liquid composite grinding aid | |
| CN102703689A (en) | Process method for extracting and separating iron from industrial waste iron mud and preparing iron oxide red | |
| CN108585721A (en) | Electrolytic manganese residues and steel slag tailing slurry comprehensive resource utilize method | |
| CN104402286B (en) | A kind of concrete early strength agent and preparation method thereof | |
| CN104610193A (en) | Preparation method of rubber vulcanizing accelerator TBBS | |
| CN104386752A (en) | Method for preparing chromium sulfate basic by utilizing residual liquor obtained during menadione production | |
| CN109824285B (en) | Cement flue gas desulfurizer and application thereof | |
| CN103539759A (en) | Method for reducing water used in synthesis process of accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) | |
| CN102838561A (en) | Production method of rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) | |
| CN103539758A (en) | Method for reducing water used in synthesis process of accelerator CBS (N-cyclohexyl-2-benzothiazole sulfenamide) | |
| CN101343257A (en) | Process for preparing rubber accelerator TBBS | |
| CN103553407A (en) | Preparation method of cement grinding aid | |
| CN105329952A (en) | Refining method of titanium dioxide by-product ferrous sulfate | |
| CN104230843A (en) | Process for sectional oxosynthesis of DM (dibenzothiazyl disulfide) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140129 |