CN113512061A - Preparation method of phosphate - Google Patents
Preparation method of phosphate Download PDFInfo
- Publication number
- CN113512061A CN113512061A CN202110974964.6A CN202110974964A CN113512061A CN 113512061 A CN113512061 A CN 113512061A CN 202110974964 A CN202110974964 A CN 202110974964A CN 113512061 A CN113512061 A CN 113512061A
- Authority
- CN
- China
- Prior art keywords
- nitrogen
- phosphorus
- reaction kettle
- filling
- preparation
- 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
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 9
- 239000010452 phosphate Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 5
- -1 phosphate ester Chemical class 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 239000011574 phosphorus Substances 0.000 claims abstract description 5
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 238000011049 filling Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 10
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 4
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 claims description 4
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 3
- 230000032050 esterification Effects 0.000 abstract 1
- 238000005886 esterification reaction Methods 0.000 abstract 1
- 239000010687 lubricating oil Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012208 gear oil Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
-
- 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
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6571—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
- C07F9/6574—Esters of oxyacids of phosphorus
- C07F9/65742—Esters of oxyacids of phosphorus non-condensed with carbocyclic rings or heterocyclic rings or ring systems
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M137/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus
- C10M137/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing phosphorus having no phosphorus-to-carbon bond
- C10M137/04—Phosphate esters
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
Abstract
The invention discloses a preparation method of phosphate ester, which is characterized by comprising the step of adding phosphorus-containing oxide into C2-C12 monohydric alcohol or polyhydric alcohol for esterification to generate the phosphate ester.
Description
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a preparation method of phosphate.
Background
The operation of equipment can not be separated from lubricating oil, lubricating oil can not be separated from a lubricating oil additive, the lubricating oil additive is the essence of various modern high-grade lubricating oil, at present, the demand for the lubricating oil in the market is large, so that the market demand for the lubricating oil additive is continuously promoted, the manufacturing cost of the lubricating oil additive in the current market is high, the production steps are complex, the extreme pressure anti-wear property and the anti-wear property of the lubricating oil additive can not meet the requirements of high-precision products, and more pollution can be generated in the preparation process, so that a preparation method of phosphate ester is designed to solve the problems.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a preparation method of phosphate, which can reduce production steps and production cost, does not generate redundant waste materials, avoids environmental pollution, and can meet the requirements of gear oil for high-grade vehicles with good extreme pressure anti-wear performance and current requirements.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of phosphate ester comprises the following steps;
s1: preparing a reaction kettle with a condensation reflux device, a thermometer, a sealed stirring rod and a nitrogen filling device;
s2: and (2) adding C2-C12 monohydric alcohol or polyhydric alcohol into the reaction kettle, stirring at room temperature under the protection of nitrogen, stopping nitrogen filling, adding phosphorus-containing oxide in batches, wherein the temperature is 0-50 ℃ during feeding, continuously filling nitrogen after feeding is finished, adjusting the temperature to 60-100 ℃, and heating for 3-5 hours to obtain the product.
Preferably, in the S2, the C2-C12 monohydric or polyhydric alcohol may be one or more of butanol, pentanol, hexanol, heptanol, octanol, nonanol, decanol, lauryl alcohol, ethylene glycol, propylene glycol, butylene glycol, and the like.
Preferably, in S2, the nitrogen charging protection is performed by nitrogen charging under liquid level.
Preferably, in S2, the phosphorus-containing oxide may be phosphorus pentoxide, phosphorus oxychloride or the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention has reasonable design, can reduce production steps and production cost, does not generate excessive waste materials, avoids environmental pollution, can meet the requirements of high-grade automobile gear oil with good extreme pressure wear resistance, and meets the current requirements.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, 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
Comprises the following steps;
s1: preparing a reaction kettle with a condensation reflux device, a thermometer, a sealed stirring rod and a nitrogen filling device;
s2: and (2) putting 306g of hexanol into the reaction kettle, stirring at room temperature under the protection of nitrogen, stopping filling nitrogen, then putting 141g of phosphorus pentoxide in batches, wherein the temperature is 0-50 ℃ during feeding, continuing filling nitrogen after feeding is finished, adjusting the temperature to 90-100 ℃, and heating for 4 hours to react to obtain the product.
Example 2
Comprises the following steps;
s1: preparing a reaction kettle with a condensation reflux device, a thermometer, a sealed stirring rod and a nitrogen filling device;
s2: and (2) putting 148g of n-butyl alcohol and 186g of lauryl alcohol into the reaction kettle, stirring at room temperature under the protection of nitrogen, stopping nitrogen filling, putting 141g of phosphorus pentoxide in batches, wherein the temperature is 0-50 ℃ during feeding, continuing nitrogen filling after feeding is finished, adjusting the temperature to 90-100 ℃, and heating for 5 hours to obtain the product.
Example 3
Comprises the following steps;
s1: preparing a reaction kettle with a condensation reflux device, a thermometer, a sealed stirring rod and a nitrogen filling device;
s2: putting 180g of butanediol into the reaction kettle, stirring at room temperature under the protection of nitrogen, stopping filling nitrogen, putting 141g of phosphorus pentoxide in batches, wherein the temperature is 0-30 ℃ during feeding, continuing filling nitrogen after feeding is finished, adjusting the temperature to 85-90 ℃, and heating for 4 hours to obtain the product.
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 (4)
1. A preparation method of phosphate ester is characterized by comprising the following steps;
s1: preparing a reaction kettle with a condensation reflux device, a thermometer, a sealed stirring rod and a nitrogen filling device;
s2: and (2) adding C2-C12 monohydric alcohol or polyhydric alcohol into the reaction kettle, stirring at room temperature under the protection of nitrogen, stopping nitrogen filling, adding phosphorus-containing oxide in batches, wherein the temperature is 0-50 ℃ during feeding, continuously filling nitrogen after feeding is finished, adjusting the temperature to 60-100 ℃, and heating for 3-5 hours to obtain the product.
2. The method of claim 1, wherein in the step of S2, the C2-C12 mono-or polyhydric alcohol is one or more selected from butanol, pentanol, hexanol, heptanol, octanol, nonanol, decanol, lauryl alcohol, ethylene glycol, propylene glycol, butylene glycol, etc.
3. The method according to claim 1, wherein in step S2, nitrogen is filled under the liquid surface for protection.
4. The method according to claim 1, wherein the phosphorus-containing oxide in S2 is phosphorus pentoxide or phosphorus oxychloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110974964.6A CN113512061A (en) | 2021-08-24 | 2021-08-24 | Preparation method of phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110974964.6A CN113512061A (en) | 2021-08-24 | 2021-08-24 | Preparation method of phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113512061A true CN113512061A (en) | 2021-10-19 |
Family
ID=78069166
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110974964.6A Pending CN113512061A (en) | 2021-08-24 | 2021-08-24 | Preparation method of phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113512061A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733874A (en) * | 2004-08-13 | 2006-02-15 | 抚顺市雷特化工科技有限公司 | Oil additive preparation method |
| CN102911203A (en) * | 2012-10-25 | 2013-02-06 | 浙江合诚化学有限公司 | Preparation method of alkyl phosphate |
| CN103833785A (en) * | 2013-12-23 | 2014-06-04 | 华南师范大学 | Synthetic method for phosphate ester |
| CN104177406A (en) * | 2013-05-22 | 2014-12-03 | 中国石油化工股份有限公司 | Bis-phosphite, preparation method and application and lubricating oil composition |
| CN110257130A (en) * | 2019-07-10 | 2019-09-20 | 新乡市瑞丰新材料股份有限公司 | A kind of preparation method of acid phosphate amine salt |
| CN112409403A (en) * | 2020-10-28 | 2021-02-26 | 成都市科宏达新材料有限公司 | Synthetic method of phosphate |
-
2021
- 2021-08-24 CN CN202110974964.6A patent/CN113512061A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733874A (en) * | 2004-08-13 | 2006-02-15 | 抚顺市雷特化工科技有限公司 | Oil additive preparation method |
| CN102911203A (en) * | 2012-10-25 | 2013-02-06 | 浙江合诚化学有限公司 | Preparation method of alkyl phosphate |
| CN104177406A (en) * | 2013-05-22 | 2014-12-03 | 中国石油化工股份有限公司 | Bis-phosphite, preparation method and application and lubricating oil composition |
| CN103833785A (en) * | 2013-12-23 | 2014-06-04 | 华南师范大学 | Synthetic method for phosphate ester |
| CN110257130A (en) * | 2019-07-10 | 2019-09-20 | 新乡市瑞丰新材料股份有限公司 | A kind of preparation method of acid phosphate amine salt |
| CN112409403A (en) * | 2020-10-28 | 2021-02-26 | 成都市科宏达新材料有限公司 | Synthetic method of phosphate |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211019 |
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| RJ01 | Rejection of invention patent application after publication |