CN110551155A - Synthetic method of organic molybdenum additive - Google Patents
Synthetic method of organic molybdenum additive Download PDFInfo
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- CN110551155A CN110551155A CN201910697516.9A CN201910697516A CN110551155A CN 110551155 A CN110551155 A CN 110551155A CN 201910697516 A CN201910697516 A CN 201910697516A CN 110551155 A CN110551155 A CN 110551155A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic System
- C07F11/005—Compounds containing elements of Groups 6 or 16 of the Periodic System compounds without a metal-carbon linkage
Abstract
The invention discloses a synthetic method of an organic molybdenum additive, belonging to the field of synthesis of dialkyl dithiocarbamate, and now proposes the following scheme, which comprises the following steps of S1, adding 1 part by weight equivalent of molybdenum trioxide powder and 1.0-1.2 parts by weight equivalent of dialkyl amine into 3.0-4.0 parts by weight of solvent A under mechanical stirring, and reacting at 20-50 ℃ to prepare an intermediate; s2, adding 1.52 parts by weight of solvent B, slowly dropwise adding 3.0-4.5 parts by weight of carbon disulfide, controlling the dropwise adding temperature at 10-35 ℃, heating the mixture to 50-120 ℃ after the dropwise adding is finished, reacting for 2-7 hours, recovering ethanol and generated water under reduced pressure for reuse, and filtering to obtain oily liquid. The synthetic process does not produce a large amount of salt-containing wastewater, does not need a matched salt-containing wastewater treatment device, has low production cost, does not cause pollution to the environment, and is suitable for popularization and use.
Description
Technical Field
The invention relates to the technical field of synthesis of dialkyl dithiocarbamate, in particular to a synthesis method of an organic molybdenum additive.
Background
Dihydrocarbyl dithiocarbamates are a multi-effect additive, have good extreme pressure properties in addition to antioxidant, anticorrosive and antiwear effects, and are typical products of molybdenum dihydrocarbyl dithiocarbamates (MoDTC). The MoDTC contains polar atoms such as sulfur, oxygen, nitrogen and the like, can be compatible with the metal surface, and forms a lubricating film of substances such as molybdenum disulfide, ferrous sulfide, ferrous oxide and the like at high temperature and high pressure, thereby generating the effects of abrasion resistance and extreme pressure. In addition, the oxidation resistance is improved due to the existence of sulfur, and meanwhile, the MoDTC decomposition process is a heat absorption process, so that heat generated due to friction can be absorbed, and the effects of reducing the oil temperature and delaying oxidation are achieved.
Through search, the hexavalent molybdenum source, dialkyl amine and carbon disulfide are generally used as raw materials and prepared by a fractional step method, and a common method is described in a patent EP 0727429: and reacting the molybdenum oxide with a sodium hydrosulfide solution, and then adding sodium hydrosulfite to continue reacting to obtain an intermediate. And adding methanol and diisooctylamine into the intermediate, dropwise adding carbon disulfide, acidifying with sulfuric acid, and filtering to obtain the product. The prior art complex operation, the in-process has a large amount of waste water to produce, contains salt waste water, needs supporting salt effluent treatment plant that contains, and manufacturing cost is high, is unfavorable for the environmental protection.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a synthetic method of an organic molybdenum additive.
In order to achieve the purpose, the invention adopts the following technical scheme:
A method for synthesizing organic molybdenum additive includes the following steps,
S1, adding 1 part by weight equivalent of molybdenum trioxide powder and 1.0-1.2 parts by weight equivalent of dialkyl amine into 3.0-4.0 parts by weight of solvent A under mechanical stirring, and reacting at 20-50 ℃ to obtain an intermediate;
S2, adding 1.52 parts by weight of solvent B, slowly dropwise adding 3.0-4.5 parts by weight of carbon disulfide, controlling the dropwise adding temperature at 10-35 ℃, heating the mixture to 50-120 ℃ after the dropwise adding is finished, reacting for 2-7 hours, recovering ethanol and generated water under reduced pressure for reuse, and filtering to obtain oily liquid.
Preferably, the ratio of the molybdenum trioxide, the dialkyl amine and the carbon disulfide is 1:1.05: 4.
Preferably, the solvent A and the solvent B are both organic solvents, mineral oils or synthetic oils.
Preferably, the solvent A and the solvent B are ethanol, toluene, xylene and 150SN base oil.
Preferably, the dihydrocarbylamine can be a single component or can be a mixture of two different dihydrocarbylamines.
Preferably, the dialkyl amine is diethylamine, dioctylamine, dipropylamine, dipentylamine, di-n-butylamine, diisobutylamine or dibenzylamine.
Preferably, the product has the following structural formula:
r 1 and R 2 can be the same group, can also be partially the same group, and even can be different groups.
Compared with the prior art, the invention has the beneficial effects that: the synthetic process does not produce a large amount of salt-containing wastewater, does not need a matched salt-containing wastewater treatment device, has low production cost, does not cause pollution to the environment, and is suitable for popularization and use.
Detailed Description
the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
the invention provides a synthetic method of an organic molybdenum additive, which comprises the steps of adding 2.88g of molybdenum trioxide, 3.6g of distilled water, 4.83g of dioctylamine and 10g of ethanol into a reaction bottle under mechanical stirring, stirring for about 2 hours at room temperature until the mixture is clear, adding 4.4g of 150SN base oil, cooling to 10-20 ℃, slowly dropwise adding 6.08g of carbon disulfide, reacting for two hours at 20-40 ℃, reacting for 5 hours at 90-110 ℃, recovering ethanol and generated water under reduced pressure for reuse, and filtering to obtain oily liquid, wherein the yield is 92.1%.
In this embodiment, the product has the following structural formula:
R 1 and R 2 can be the same group, can also be partially the same group, and even can be different groups.
Example 2
The invention provides a synthetic method of an organic molybdenum additive, which comprises the steps of adding 2.73g of molybdenum trioxide, 3.45g of distilled water, 4.67g of dioctylamine and 9g of ethanol into a reaction bottle under mechanical stirring, stirring for about 2 hours at room temperature until the mixture is clear, adding 4.25g of 150SN base oil, cooling to 10-25 ℃, slowly dropwise adding 6.04g of carbon disulfide, reacting for two hours at 20-35 ℃, reacting for 5.5 hours at 60-110 ℃, recovering ethanol and generated water under reduced pressure for reuse, and filtering to obtain oily liquid with the yield of 90.8%.
in this embodiment, the product has the following structural formula:
r 1 and R 2 can be the same group, can also be partially the same group, and even can be different groups.
Example 3
The invention provides a synthetic method of an organic molybdenum additive, which comprises the steps of adding 2.93g of molybdenum trioxide, 3.71g of distilled water, 4.88g of dioctylamine and 11g of ethanol into a reaction bottle under mechanical stirring, stirring for about 2 hours at room temperature until the mixture is clear, adding 4.5g of 150SN base oil, cooling to 10-20 ℃, slowly dropwise adding 6.15g of carbon disulfide, reacting for two hours at 25-40 ℃, reacting for 6 hours at 80-100 ℃, recovering ethanol and generated water under reduced pressure for reuse, and filtering to obtain oily liquid, wherein the yield is 91.7%.
In this embodiment, the product has the following structural formula:
R 1 and R 2 can be the same group, can also be partially the same group, and even can be different groups.
the synthetic process does not produce a large amount of salt-containing wastewater, does not need a matched salt-containing wastewater treatment device, has low production cost, does not cause pollution to the environment, and is suitable for popularization and use.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A method for synthesizing an organic molybdenum additive is characterized by comprising the following steps,
S1, adding 1 part by weight equivalent of molybdenum trioxide powder and 1.0-1.2 parts by weight equivalent of dialkyl amine into 3.0-4.0 parts by weight of solvent A under mechanical stirring, and reacting at 20-50 ℃ to obtain an intermediate;
s2, adding 1.52 parts by weight of solvent B, slowly dropwise adding 3.0-4.5 parts by weight of carbon disulfide, controlling the dropwise adding temperature at 10-35 ℃, heating the mixture to 50-120 ℃ after the dropwise adding is finished, reacting for 2-7 hours, recovering ethanol and generated water under reduced pressure for reuse, and filtering to obtain oily liquid.
2. The method of synthesizing an organomolybdenum additive as claimed in claim 1, wherein the ratio of molybdenum trioxide, dihydrocarbylamine, and carbon disulfide is 1:1.05: 4.
3. the method for synthesizing organic molybdenum additive according to claim 1, wherein the solvent A and the solvent B are both organic solvent, mineral oil or synthetic oil.
4. The method for synthesizing organic molybdenum additive according to claim 3, wherein the solvent A and the solvent B are ethanol, toluene, xylene, 150SN base oil.
5. The method of claim 1, wherein the dialkyl amine is a single component or a mixture of two different dialkyl amines.
6. The method for synthesizing organic molybdenum additive according to claim 5, wherein the dialkyl amine is diethylamine, dioctylamine, dipropylamine, dipentylamine, di-n-butylamine, diisobutylamine or dibenzylamine.
7. The method for synthesizing the organo-molybdenum additive according to any one of claims 1 to 6 wherein the product has the following structural formula:
R 1 and R 2 can be the same group, can also be partially the same group, and even can be different groups.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0638582A2 (en) * | 1993-08-13 | 1995-02-15 | Asahi Denka Kogyo Kabushiki Kaisha | A powdery molybdenum oxysulfide dithiocarbamate composition, a process for producing same, and a grease composition containing the composition |
| CN101137739A (en) * | 2005-03-01 | 2008-03-05 | R.T.范德比尔特公司 | Molybdenum dialkyldithiocarbamate compositions and lubricating compositions containing the same |
| CN108504416A (en) * | 2018-03-27 | 2018-09-07 | 新乡市瑞丰新材料股份有限公司 | The preparation method of carbamic acid molybdenum lube oil additive |
-
2019
- 2019-07-30 CN CN201910697516.9A patent/CN110551155A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0638582A2 (en) * | 1993-08-13 | 1995-02-15 | Asahi Denka Kogyo Kabushiki Kaisha | A powdery molybdenum oxysulfide dithiocarbamate composition, a process for producing same, and a grease composition containing the composition |
| CN101137739A (en) * | 2005-03-01 | 2008-03-05 | R.T.范德比尔特公司 | Molybdenum dialkyldithiocarbamate compositions and lubricating compositions containing the same |
| CN108504416A (en) * | 2018-03-27 | 2018-09-07 | 新乡市瑞丰新材料股份有限公司 | The preparation method of carbamic acid molybdenum lube oil additive |
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Application publication date: 20191210 |