CN110483355A - The synthetic method of dialkyldithiocarbamates zinc salt - Google Patents
The synthetic method of dialkyldithiocarbamates zinc salt Download PDFInfo
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- CN110483355A CN110483355A CN201910696979.3A CN201910696979A CN110483355A CN 110483355 A CN110483355 A CN 110483355A CN 201910696979 A CN201910696979 A CN 201910696979A CN 110483355 A CN110483355 A CN 110483355A
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- Prior art keywords
- dialkyldithiocarbamates
- zinc salt
- synthetic method
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
- C07C333/16—Salts of dithiocarbamic acids
Abstract
The invention discloses the synthetic methods of dialkyldithiocarbamates zinc salt, belong to the synthesis field of dialkyldithiocarbamates zinc salt, now propose following scheme, it includes the following steps, S1, under mechanical stirring, the Powder Oxidation zinc and 2.0-2.5 parts by weight equivalent dialkyl amine of 1 parts by weight equivalent are added in the solvent of 60-100 parts by weight, then the equivalent carbon disulfide of 2.0-2.5 parts by weight is slowly added dropwise；S2 is stirred the mixture for 1-12 hours, heats 50-95 DEG C, the water generated in reaction process is mixed object filtering finally by vacuum distillation removing to get required product.A large amount of brine waste will not be generated in synthesis process of the present invention, does not need mating salt-containing waste water treating device, and production cost is low, not can cause environmental pollution, and is suitble to promote the use of.
Description
Technical field
The present invention relates to the synthesis technical field of dialkyldithiocarbamates zinc salt more particularly to dihydrocarbyl dithiophosphates
The synthetic method of carbamic acid zinc salt.
Background technique
Dialkyldithiocarbamates salt is a kind of multipurpose additive, in addition to going back with antioxygen, anti-rotten and wear-resistant effect
Preferable extreme pressure property is had both, dialkyldithiocarbamates zinc (ZDTC) is the typical product of one type.
The usually synthesis common method of dialkyldithiocarbamates zinc is mainly step synthesis.Substep synthesis technology
A large amount of brine waste is generated in the process, needs mating salt-containing waste water treating device, and high production cost easily causes environmental pollution.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and the dihydrocarbyl dithiophosphate amino first proposed
The synthetic method of sour zinc salt.
To achieve the goals above, present invention employs following technical solutions:
The synthetic method of dialkyldithiocarbamates zinc salt, includes the following steps,
S1, under mechanical stirring, the Powder Oxidation zinc and 2.0-2.5 parts by weight equivalent dialkyl of 1 parts by weight equivalent
Amine is added in the solvent of 60-100 parts by weight, then the equivalent carbon disulfide of 2.0-2.5 parts by weight is slowly added dropwise；
S2 is stirred the mixture for 1-12 hours, heats 50-95 DEG C, the water generated in reaction process is de- by vacuum distillation
It removes, is mixed object filtering finally to get required product.
Preferably, the zinc oxide, dialkyl amine, carbon disulfide ratio be 1:2.1:2.2, solvent be zinc oxide, two
20 times of alkylamine, carbon disulfide mixture.
Preferably, solvent uses organic solvent, mineral oil or synthetic oil.
Preferably, the solvent is toluene, dimethylbenzene, 150SN base oil.
Preferably, the dialkyl amine can be one-component, be also possible to the mixture of two different dialkyl amines.
Preferably, the dialkyl amine using diethylamine, di-n-propylamine, di-n-butyl amine, diisobutyl amine, diamylamine or
Dibenzylamine.
Preferably, the product structure formula is as follows:
R1, R2, R3, R4It can be identical group, or the identical group in part, even mutually different base
Group, R1, R2, R3, R4For one or more of ethyl, propyl, butyl, isobutyl group, amyl, benzyl.
Compared with prior art, the beneficial effects of the present invention are: will not be generated in synthesis process of the present invention a large amount of
Brine waste does not need mating salt-containing waste water treating device, and production cost is low, not can cause environmental pollution, and suitable popularization makes
With.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment
The synthetic method of dialkyldithiocarbamates zinc salt proposed by the present invention, under mechanical stirring, 1.62g
Powder Oxidation zinc and 6.6g diamyl amine are added in 32g solvent and are stirred at room temperature 2 hours, then 3.35g carbon disulfide is slowly added dropwise,
10-20 DEG C of temperature of control, after completion of dropwise addition, is warming up to 60-70 DEG C, stirs the mixture for 6 hours, the water generated in reaction process
It is removed by vacuum distillation, is mixed object filtering, finally up to required product.
Solvent uses organic solvent, mineral oil or synthetic oil.
In present embodiment, the solvent is toluene, dimethylbenzene, 150SN base oil.
In present embodiment, the dialkyl amine can be one-component, be also possible to two different dialkyl amines
Mixture.
In present embodiment, the dialkyl amine uses diethylamine, di-n-propylamine, di-n-butyl amine, diisobutyl amine, diamyl
Amine or dibenzylamine.
In present embodiment, the product structure formula is as follows:
R1, R2, R3, R4It can be identical group, or the identical group in part, even mutually different base
Group, R1, R2, R3, R4For one or more of ethyl, propyl, butyl, isobutyl group, amyl, benzyl.
A large amount of brine waste will not be generated in synthesis process of the present invention, do not need mating brine waste processing dress
It sets, production cost is low, not can cause environmental pollution, and is suitble to promote the use of.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. the synthetic method of dialkyldithiocarbamates zinc salt, which is characterized in that include the following steps,
S1 adds the Powder Oxidation zinc and 2.0-2.5 parts by weight equivalent dialkyl amine of 1 parts by weight equivalent under mechanical stirring
In the solvent for entering 60-100 parts by weight, then the equivalent carbon disulfide of 2.0-2.5 parts by weight is slowly added dropwise；
S2 is stirred the mixture for 1-12 hours, heats 50-95 DEG C, the water generated in reaction process is by vacuum distillation removing, most
After be mixed object filtering to get required product.
2. the synthetic method of dialkyldithiocarbamates zinc salt according to claim 1, which is characterized in that the oxygen
Change zinc, dialkyl amine, carbon disulfide ratio be 1:2.1:2.2, solvent be zinc oxide, dialkyl amine, carbon disulfide mixture
20 times.
3. the synthetic method of dialkyldithiocarbamates zinc salt according to claim 1, which is characterized in that solvent is adopted
With organic solvent, mineral oil or synthetic oil.
4. the synthetic method of dialkyldithiocarbamates zinc salt according to claim 3, which is characterized in that described molten
Agent is toluene, dimethylbenzene, 150SN base oil.
5. the synthetic method of dialkyldithiocarbamates zinc salt according to claim 1, which is characterized in that described two
Alkylamine can be one-component, be also possible to the mixture of two different dialkyl amines.
6. the synthetic method of dialkyldithiocarbamates zinc salt according to claim 5, which is characterized in that described two
Alkylamine uses diethylamine, di-n-propylamine, di-n-butyl amine, diisobutyl amine, diamylamine or dibenzylamine.
7. the synthetic method of dialkyldithiocarbamates zinc salt according to claim 1 to 6, feature
It is, the product structure formula is as follows:
R1, R2, R3, R4It can be identical group, or the identical group in part, even mutually different group, R1,
R2, R3, R4For one or more of ethyl, propyl, butyl, isobutyl group, amyl, benzyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910696979.3A CN110483355A (en) | 2019-07-30 | 2019-07-30 | The synthetic method of dialkyldithiocarbamates zinc salt |
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| CN201910696979.3A CN110483355A (en) | 2019-07-30 | 2019-07-30 | The synthetic method of dialkyldithiocarbamates zinc salt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213297A (en) * | 2021-12-01 | 2022-03-22 | 蔚林新材料科技股份有限公司 | Method for continuously synthesizing rubber vulcanization accelerator EZ |
| WO2023228114A1 (en) | 2022-05-25 | 2023-11-30 | Universidad Santiago De Cali | Aromatic amine derivatives coordinated to metals as bactericidal materials and the production process thereof |
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| US2492314A (en) * | 1945-01-16 | 1949-12-27 | Sharples Chemicals Inc | Process for producing metal salts of substituted dithiocarbamic acids |
| CN102276509A (en) * | 2011-06-03 | 2011-12-14 | 鹤壁联昊化工有限公司 | One-step method for preparing rubber promoter zinc dibenzyl dithiocarbamate |
| CN105061277A (en) * | 2015-07-16 | 2015-11-18 | 山东阳谷华泰化工股份有限公司 | Environment-friendly preparation method of accelerator zinc dibenzyldithiocarbamate |
| CN105732451A (en) * | 2016-02-01 | 2016-07-06 | 武汉径河化工（潜江)有限公司 | Method for producing zinc dimethyldithiocarbamate rubber vulcanization accelerant without wastewater generation |
| CN106188699A (en) * | 2016-07-07 | 2016-12-07 | 芜湖风雪橡胶有限公司 | Flame retardant rubber composition and the preparation method of flame retardant rubber |
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2019
- 2019-07-30 CN CN201910696979.3A patent/CN110483355A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2492314A (en) * | 1945-01-16 | 1949-12-27 | Sharples Chemicals Inc | Process for producing metal salts of substituted dithiocarbamic acids |
| CN102276509A (en) * | 2011-06-03 | 2011-12-14 | 鹤壁联昊化工有限公司 | One-step method for preparing rubber promoter zinc dibenzyl dithiocarbamate |
| CN105061277A (en) * | 2015-07-16 | 2015-11-18 | 山东阳谷华泰化工股份有限公司 | Environment-friendly preparation method of accelerator zinc dibenzyldithiocarbamate |
| CN105732451A (en) * | 2016-02-01 | 2016-07-06 | 武汉径河化工（潜江)有限公司 | Method for producing zinc dimethyldithiocarbamate rubber vulcanization accelerant without wastewater generation |
| CN106188699A (en) * | 2016-07-07 | 2016-12-07 | 芜湖风雪橡胶有限公司 | Flame retardant rubber composition and the preparation method of flame retardant rubber |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213297A (en) * | 2021-12-01 | 2022-03-22 | 蔚林新材料科技股份有限公司 | Method for continuously synthesizing rubber vulcanization accelerator EZ |
| WO2023228114A1 (en) | 2022-05-25 | 2023-11-30 | Universidad Santiago De Cali | Aromatic amine derivatives coordinated to metals as bactericidal materials and the production process thereof |
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