CN113461728B - Purification method for improving hydrolysis resistance of phosphate fire-resistant oil - Google Patents
Purification method for improving hydrolysis resistance of phosphate fire-resistant oil Download PDFInfo
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- CN113461728B CN113461728B CN202111025646.1A CN202111025646A CN113461728B CN 113461728 B CN113461728 B CN 113461728B CN 202111025646 A CN202111025646 A CN 202111025646A CN 113461728 B CN113461728 B CN 113461728B
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- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 75
- 239000010452 phosphate Substances 0.000 title claims abstract description 74
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 44
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 27
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 27
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000746 purification Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 52
- 238000005406 washing Methods 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- -1 phosphate ester Chemical class 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000005484 gravity Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 7
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 11
- 239000003208 petroleum Substances 0.000 claims description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 6
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000012043 crude product Substances 0.000 abstract 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 abstract 1
- 235000021317 phosphate Nutrition 0.000 description 55
- 239000003921 oil Substances 0.000 description 29
- 239000000126 substance Substances 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- 239000010723 turbine oil Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000010720 hydraulic oil Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000004713 phosphodiesters Chemical class 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical group 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 125000003944 tolyl group Chemical group 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
- C07F9/12—Esters of phosphoric acids with hydroxyaryl compounds
-
- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/74—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing phosphorus
-
- 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
- C10M2223/041—Triaryl phosphates
- C10M2223/0415—Triaryl phosphates used as base material
-
- 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
- C10N2030/52—Base number [TBN]
-
- 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
- C10N2030/66—Hydrolytic stability
-
- 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
- C10N2040/08—Hydraulic fluids, e.g. brake-fluids
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 purification method for improving hydrolysis resistance of phosphate fire-resistant oil, belonging to the technical field of fire-resistant oil, comprising the following steps: adding a phosphate ester crude product and a solvent into a washing kettle, stirring and dissolving the phosphate ester crude product and the solvent, adding 1-5% alkaline water for alkali washing, heating and fully stirring, pumping the material into a layering tank through a centrifugal pump for standing, performing gravity settling separation, and putting the precipitated material into the washing kettle; repeatedly carrying out second alkali washing; putting the precipitate into the material in a washing kettle, adding deionized water for washing for the third time, and then carrying out layered precipitation; feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters; and finally, cooling the phosphate material, sampling and analyzing. The method is simple and convenient to operate, the phosphate crude product is dissolved by the organic solvent, and after the phosphate crude product is purified for many times by 1-5% alkaline water and deionized water, the hydrolysis stability HS of the prepared phosphate material is less than or equal to 0.05, so that the aim of improving the hydrolysis resistance of the phosphate fire-resistant oil is fulfilled.
Description
Technical Field
The invention belongs to the technical field of fire-resistant oil, and particularly relates to a purification method for improving hydrolysis resistance of phosphate fire-resistant oil.
Background
The fire-resistant oil is classified into phosphate ester, silicate ester, petroleum-based oil, water-glycol emulsion, synthetic hydrocarbon, and the like. Among them, phosphate esters widely used in turbine electrohydraulic control systems are the most commonly used, and phosphate esters are classified into 3 types of aryl phosphate esters, alkyl phosphate esters and aryl-alkyl phosphate esters according to the structure. The aryl phosphate has better hydrolytic resistance, thermal oxidation stability and flame resistance, is mainly used as flame-resistant turbine oil in power systems and in the metallurgical industry except the fields of aviation, aerospace and the like, has higher viscosity, flash point, spontaneous combustion point and thermal decomposition temperature, and can meet the requirements of a regulating system of a large-capacity turbine set on a medium. The flame-retardant heat-insulating material does not burn at a high temperature, does not spread flame even if burning occurs under conditions of high temperature and burning, and automatically extinguishes the flame after a heat source is cut off, so that burning is stopped. In a power plant, if mineral turbine oil is used, once leakage occurs and high temperature is encountered, the possibility of fire is very high, and fire is caused. And the phosphate fire-resistant oil is used as a working medium of the regulating system, so that fire caused by oil leakage can be greatly reduced.
Compared with mineral turbine oil, the phosphate fire-resistant oil has excellent fire resistance (the spontaneous combustion point is more than 530 ℃), and compared with other synthetic hydraulic fluids, the phosphate fire-resistant oil has good stability and abrasion resistance. Most of adjusting systems of the steam turbines of the power plants are close to a superheated steam pipeline (the temperature of the superheated steam is over 540 ℃), the oil pressure of the adjusting systems reaches over 14 MPa, mineral oil (the spontaneous combustion point is only about 300 ℃) is used as a hydraulic adjusting working medium, and once leakage occurs, the danger of fire is very high. According to the statistics of the German insurance company, 94% of station fires occur in the oil system of the steam turbine, of which about 49% occur in the hydraulic system and 43% occur in the lubricating system. Therefore, phosphate fire-resistant oil is widely adopted as a hydraulic working medium in the regulating system of the steam turbines in various countries in the world at present in order to improve the fire-proof capability of the power plant and reduce the fire-fighting cost.
The phosphate fire-resistant oil has stronger polarity and is easy to absorb moisture in the air. Under appropriate conditions, such as severe stirring and the presence of acidic substances, hydrolysis can occur under the action of moisture, acidic phosphodiester, acidic phosphomonoester, phenolic substances and the like can be generated to different degrees, the acidic substances generated by hydrolysis have catalytic action on further hydrolysis of oil, and phosphoric acid and phenolic substances are generated after complete hydrolysis, so that corrosion is caused to a system, and the service life of the fire-resistant oil is influenced.
In the prior art, the improvement of the hydrolytic stability of oil is mainly realized by controlling the purity of synthetic raw materials, and natural raw materials such as phosphate synthesized by alkylphenol extracted from coal tar have better hydrolytic stability; it has also been reported that the hydrolysis of oil is blocked by the addition of hydrolysis-resistant additives such as piperazine-like compounds; in addition, the water content in the oil can be strictly controlled to achieve the aim of avoiding the hydrolysis of the oil. However, the above method has problems of high cost, complex process or poor effect.
Disclosure of Invention
The invention aims to provide a purification method which reduces the cost, simplifies the operation and improves the hydrolysis resistance of phosphate ester fire-resistant oil.
In order to achieve the purpose, the invention adopts the technical scheme that: a purification method for improving hydrolysis resistance of phosphate ester fire-resistant oil comprises the following steps:
step one, adding a crude phosphate into a washing kettle;
adding a solvent into the washing kettle, wherein the mass of the solvent is 50-70% of that of the crude phosphate ester product;
step three, stirring and dissolving the crude phosphate ester and a solvent, and then adding 1-5% alkaline water for alkaline washing, wherein the mass of the 1-5% alkaline water is 60-90% of that of the crude phosphate ester;
step four, heating to 40-65 ℃, stirring fully, pumping the materials into a layering tank through a centrifugal pump for standing, performing gravity settling separation, draining a water layer, and putting the precipitated materials into a washing kettle;
step five, repeating the step three and the step four to carry out secondary alkali washing;
sixthly, putting the precipitate obtained in the fifth step into a material of a washing kettle, adding deionized water into the material to carry out third washing, wherein the mass of the deionized water is 60-90% of that of the crude phosphate product, and then repeating the fourth step to carry out layered precipitation;
step seven, feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters to obtain a purified phosphate ester material;
and step eight, cooling the phosphate material to 80 ℃, and sampling and analyzing.
In step one, the phosphate ester is a triaryl phosphate ester.
In the second step, the solvent is one or two of toluene, xylene, cyclohexane, methylcyclohexane, petroleum ether at 30-60 ℃, petroleum ether at 60-90 ℃, petroleum ether at 90-120 ℃, octanol, decanol and solvent oil.
The hydrolytic stability HS of the phosphate material is less than or equal to 0.05.
Due to the adoption of the technical scheme, the operation is simple and convenient, after the crude triaryl phosphate is fully dissolved and dispersed by the organic solvent, phenolic substances are removed through 1-5% alkaline water in a gradient manner, and the deionized water is used for removing cations for multiple purification treatments, so that the hydrolysis stability HS of the prepared triaryl phosphate material is less than or equal to 0.05 and is far lower than the qualified standard that the hydrolysis stability HS is less than or equal to 0.5 specified in the standard DL/T571-2014 of the people's republic of China, and the purpose of improving the hydrolysis resistance of the phosphate fire-resistant oil is realized.
Detailed Description
The invention is further described with reference to the following examples:
phosphate ester fire-resistant oil is a synthetic hydraulic oil, some characteristics of which are quite different from those of mineral oil, and phosphate ester is a fire-resistant hydraulic oil which is more commonly used. Commonly used are tertiary phosphates of the general formula (RO)3And P ═ O, wherein three R groups in the general formula are all aromatic groups, is triaryl phosphate, and the phosphate referred to herein is triaryl phosphate.
Example 1:
a purification method for improving hydrolysis resistance of phosphate ester fire-resistant oil comprises the following steps:
step one, adding 3kg of crude phosphate into a washing kettle;
step two, adding 2kg of solvent into the washing kettle, wherein the solvent is toluene and cyclohexane, and the weight ratio of toluene: cyclohexane =1: 1;
step three, stirring and dissolving the crude phosphate and a solvent, and adding 2kg of 3% alkaline water for alkaline washing;
step four, heating to 50-55 ℃, stirring fully, pumping the materials into a layering tank through a centrifugal pump for standing, performing gravity settling separation, draining a water layer, and putting the precipitated materials into a washing kettle;
step five, repeating the step three and the step four to carry out secondary alkali washing;
step six, putting the precipitate obtained in the step five into the material in a washing kettle, adding 2kg of deionized water into the material to carry out third washing, and then repeating the step four to carry out layered precipitation;
step seven, feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters to obtain a purified phosphate ester material;
and step eight, cooling the phosphate material to 80 ℃, and sampling and analyzing.
Example 2:
a purification method for improving hydrolysis resistance of phosphate ester fire-resistant oil comprises the following steps:
step one, adding 3kg of crude phosphate into a washing kettle;
step two, adding 1.6kg of solvent into the washing kettle, wherein the solvent is petroleum ether at the temperature of 60-90 ℃;
step three, stirring and dissolving the crude phosphate and a solvent, and then adding 2kg of 2% alkaline water for alkaline washing;
step four, heating to 40-45 ℃, stirring fully, pumping the materials into a layering tank through a centrifugal pump for standing, performing gravity settling separation, draining a water layer, and putting the precipitated materials into a washing kettle;
step five, repeating the step three and the step four to carry out secondary alkali washing;
step six, putting the precipitate obtained in the step five into the material in a washing kettle, adding 2kg of deionized water into the material to carry out third washing, and then repeating the step four to carry out layered precipitation;
step seven, feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters to obtain a purified phosphate ester material;
and step eight, cooling the phosphate material to 80 ℃, and sampling and analyzing.
Example 3:
a purification method for improving hydrolysis resistance of phosphate ester fire-resistant oil comprises the following steps:
step one, adding 3kg of crude phosphate into a washing kettle;
step two, adding 2.1kg of solvent into the washing kettle, wherein the solvent is dimethylbenzene;
step three, stirring and dissolving the crude phosphate and the solvent, and then adding 1.8kg of 4% alkaline water for alkaline washing;
step four, heating to 60-65 ℃, stirring fully, pumping the materials into a layering tank through a centrifugal pump for standing, performing gravity settling separation, draining a water layer, and putting the precipitated materials into a washing kettle;
step five, repeating the step three and the step four to carry out secondary alkali washing;
step six, putting the precipitate obtained in the step five into the material in a washing kettle, adding 1.8kg of deionized water into the material to carry out third washing, and then repeating the step four to carry out layered precipitation;
step seven, feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters to obtain a purified phosphate ester material;
and step eight, cooling the phosphate material to 80 ℃, and sampling and analyzing.
Example 4:
a purification method for improving hydrolysis resistance of phosphate ester fire-resistant oil comprises the following steps:
step one, adding 3kg of crude phosphate into a washing kettle;
step two, adding 1.9kg of solvent into the washing kettle, wherein the solvent is methylcyclohexane;
step three, stirring and dissolving the crude phosphate and the solvent, and then adding 2.1kg of 5% alkaline water for alkaline washing;
step four, heating to 50-55 ℃, stirring fully, pumping the materials into a layering tank through a centrifugal pump for standing, performing gravity settling separation, draining a water layer, and putting the precipitated materials into a washing kettle;
step five, repeating the step three and the step four to carry out secondary alkali washing;
step six, putting the precipitate obtained in the step five into the material in a washing kettle, adding 2.1kg of deionized water into the material to carry out third washing, and then repeating the step four to carry out layered precipitation;
step seven, feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters to obtain a purified phosphate ester material;
and step eight, cooling the phosphate material to 80 ℃, and sampling and analyzing.
The phosphate material samples of examples 1-4 were analyzed to obtain the following monitoring data for hydrolytic stability:
TABLE 1 hydrolysis stability monitoring data
The method is simple and convenient to operate, after the crude triaryl phosphate is fully dissolved and dispersed by the organic solvent, phenolic substances are removed through 1-5% alkaline water gradient, and the deionized water is used for removing cations for multiple purification treatments, so that the hydrolysis stability HS of the prepared triaryl phosphate is less than or equal to 0.05 and is far lower than the qualified standard that the hydrolysis stability HS is less than or equal to 0.5 specified in the standard DL/T571-2014 of the power industry of the people's republic of China, and the purpose of improving the hydrolysis resistance of phosphate fire-resistant oil is achieved.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention should be covered by the present patent.
Claims (1)
1. A purification method for improving hydrolysis resistance of phosphate ester fire-resistant oil is characterized by comprising the following steps: the method comprises the following steps:
step one, adding a crude phosphate into a washing kettle;
step two, adding a solvent into the washing kettle, wherein the mass of the solvent is 50-70% of that of the crude phosphate ester product; in the second step, the solvent is one of toluene, xylene, cyclohexane, methylcyclohexane, petroleum ether at 30-60 ℃, petroleum ether at 60-90 ℃, petroleum ether at 90-120 ℃, octanol, decanol and solvent oil;
step three, stirring and dissolving the crude phosphate ester and a solvent, and then adding 1-5% alkaline water for alkaline washing, wherein the mass of the 1-5% alkaline water is 60-90% of that of the crude phosphate ester;
step four, heating to 40-65 ℃, stirring fully, pumping the materials into a layering tank through a centrifugal pump for standing, performing gravity settling separation, draining a water layer, and putting the precipitated materials into a washing kettle;
step five, repeating the step three and the step four to carry out secondary alkali washing;
sixthly, putting the precipitate obtained in the fifth step into a material of a washing kettle, adding deionized water into the material to carry out third washing, wherein the mass of the deionized water is 60-90% of that of the crude phosphate product, and then repeating the fourth step to carry out layered precipitation;
step seven, feeding the washed precipitate material into a wiped film evaporator, and evaporating the solvent, water and volatile matters to obtain a purified phosphate ester material; cooling the phosphate ester material purified in the step seven to 80 ℃, and sampling and analyzing;
the hydrolytic stability HS of the phosphate material is less than or equal to 0.05;
the phosphate ester is triaryl phosphate ester.
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| US3010907A (en) * | 1957-04-09 | 1961-11-28 | Pennsalt Chemicals Corp | Alkaline cleaning compositions |
| US6399685B1 (en) * | 2000-12-11 | 2002-06-04 | Albemarle Corporation | Purification of arylene polyphosphate esters |
| CN105859769B (en) * | 2015-01-23 | 2018-11-09 | 浙江新安化工集团股份有限公司 | It is a kind of to reduce the phosphate flame retardant after-treatment device and method that waste water generates |
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