CN115838611A - Composite cleaning agent for cleaning phosphate fire-resistant oil system and preparation method thereof - Google Patents
Composite cleaning agent for cleaning phosphate fire-resistant oil system and preparation method thereof Download PDFInfo
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- CN115838611A CN115838611A CN202211537429.5A CN202211537429A CN115838611A CN 115838611 A CN115838611 A CN 115838611A CN 202211537429 A CN202211537429 A CN 202211537429A CN 115838611 A CN115838611 A CN 115838611A
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- 239000012459 cleaning agent Substances 0.000 title claims abstract description 78
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 71
- 239000010452 phosphate Substances 0.000 title claims abstract description 71
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 62
- 238000004140 cleaning Methods 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 53
- -1 phosphate ester Chemical class 0.000 claims abstract description 37
- 239000002270 dispersing agent Substances 0.000 claims abstract description 31
- 239000003223 protective agent Substances 0.000 claims abstract description 21
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 53
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 claims description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- ZTOKUMPYMPKCFX-CZNUEWPDSA-N (E)-17-[(2R,3R,4S,5S,6R)-6-(acetyloxymethyl)-3-[(2S,3R,4S,5S,6R)-6-(acetyloxymethyl)-3,4,5-trihydroxyoxan-2-yl]oxy-4,5-dihydroxyoxan-2-yl]oxyoctadec-9-enoic acid Chemical compound OC(=O)CCCCCCC/C=C/CCCCCCC(C)O[C@@H]1O[C@H](COC(C)=O)[C@@H](O)[C@H](O)[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](COC(C)=O)O1 ZTOKUMPYMPKCFX-CZNUEWPDSA-N 0.000 claims description 14
- 239000003637 basic solution Substances 0.000 claims description 14
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000008096 xylene Substances 0.000 claims description 12
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 11
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 10
- 239000002585 base Substances 0.000 claims description 10
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 10
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 9
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 8
- 150000002596 lactones Chemical class 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 150000008301 phosphite esters Chemical class 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000004982 aromatic amines Chemical class 0.000 claims description 6
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical class C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 claims description 4
- QAPVYZRWKDXNDK-UHFFFAOYSA-N P,P-Dioctyldiphenylamine Chemical compound C1=CC(CCCCCCCC)=CC=C1NC1=CC=C(CCCCCCCC)C=C1 QAPVYZRWKDXNDK-UHFFFAOYSA-N 0.000 claims description 4
- 238000005691 oxidative coupling reaction Methods 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims 4
- 239000000203 mixture Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 6
- 238000011010 flushing procedure Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 84
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- 239000002184 metal Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 8
- 239000010802 sludge Substances 0.000 description 8
- 239000000295 fuel oil Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- FCBUKWWQSZQDDI-UHFFFAOYSA-N rhamnolipid Chemical compound CCCCCCCC(CC(O)=O)OC(=O)CC(CCCCCCC)OC1OC(C)C(O)C(O)C1OC1C(O)C(O)C(O)C(C)O1 FCBUKWWQSZQDDI-UHFFFAOYSA-N 0.000 description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Images
Abstract
The invention belongs to the technical field of cleaning agents, and discloses a composite cleaning agent for cleaning a phosphate ester fire-resistant oil system and a preparation method thereof, wherein the composite cleaning agent comprises triaryl phosphate ester, a cleaning agent, a dispersing agent, a defoaming agent and a protective agent; the dosage of the cleaning agent is 5-16% of the total weight of the triaryl phosphate and the dispersing agent, the dosage of the defoaming agent is 0.5-1.6% of the total weight of the triaryl phosphate and the dispersing agent, and the dosage of the protective agent is 11-31% of the total weight of the triaryl phosphate and the dispersing agent. Mixing the dispersing agent and the triaryl phosphate, adding the cleaning agent, stirring uniformly, adding the defoaming agent, stirring until the mixture is clear, adding the protective agent, and stirring until the mixture is clear. The composite cleaning agent can solve the problems of energy waste caused by the residual cleaning agent from chemical cleaning to pollute a new oil changing and oil system, the need of using a large amount of phosphate ester fire resistant oil for flushing and replacement and the like, and has the advantages of reducing corrosion and jamming of a servo valve and improving the cooling effect of an oil cooler of the oil system.
Description
Technical Field
The invention relates to a cleaning agent and a preparation method thereof, in particular to a composite cleaning agent for cleaning a phosphate ester fire-resistant oil system and a preparation method thereof.
Background
The phosphate fire-resistant oil has excellent heat-resistant and fire-resistant performance and lubricating performance, and is widely used in a speed regulating system of a steam turbine.
The phosphate ester fire-resistant oil is a phosphate ester synthetic liquid, compared with other oil products, the phosphate ester fire-resistant oil is high in degradation speed, oil sludge and other aging products can be generated after the phosphate ester fire-resistant oil is used for a period of time, the acid value of the fire-resistant oil is increased, foams are increased, the oil sludge can be deposited in an oil system, the action flexibility of a steam turbine adjusting part sleeve is reduced, a servo valve of a speed regulating system is corroded and jammed, and abnormal shutdown accidents of a unit can occur in severe cases.
Therefore, when the anti-fuel oil is seriously degraded and the oil sludge is separated out, the anti-fuel oil system needs to be thoroughly cleaned to remove the oil sludge adhered to the oil system and other degradation products, and then the qualified oil product is replaced to continue running.
The cleaning mode of the existing anti-fuel oil system is chemical cleaning, the cleaning agent is mostly a water-soluble polar cleaning agent, after the cleaning agent is cleaned, a large amount of demineralized water is needed to replace the residual cleaning agent, then the demineralized water is discharged, phosphate ester anti-fuel oil is adopted as flushing oil to flush for a plurality of times so as to replace the water in the system, because water and oil are amphoteric substances, the former is polar, the latter is nonpolar, the solubility of the two is poor, the flushing replacement process after the cleaning is finished is caused, even if a large amount of anti-fuel oil is adopted to flush and replace, the residual water in the oil system can not be completely replaced.
At present, due to the fact that a fire-resistant oil system is cleaned, trace polar cleaning agents and water are left, oil product degradation is caused, and large-area faults of a servo valve occur sometimes. Therefore, the chemical cleaning mode and the formula of the cleaning agent for the commonly used fire-resistant oil system not only can waste a large amount of phosphate fire-resistant oil and cause great economic loss to users, but also can easily cause the fault of the speed regulating system due to the residual cleaning agent and moisture after cleaning and influence the safe operation of the unit.
Disclosure of Invention
In order to solve the problems of oil product degradation and large-area failure of a servo valve caused by the fact that a large amount of expensive fire-resistant oil is wasted and polar cleaning agents and water are left in an oil system during cleaning in the prior art, the invention aims to provide the composite cleaning agent for cleaning the phosphate fire-resistant oil system and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a composite cleaning agent for cleaning a phosphate ester fire-resistant oil system comprises triaryl phosphate ester, a cleaning agent, a dispersing agent, a defoaming agent and a protective agent; wherein, the dosage of the cleaning agent is 5 to 16 percent of the total weight of the triaryl phosphate and the dispersant, the dosage of the defoaming agent is 0.5 to 1.6 percent of the total weight of the triaryl phosphate and the dispersant, and the dosage of the protective agent is 11 to 31 percent of the total weight of the triaryl phosphate and the dispersant.
Furthermore, the dosage of the dispersant is 6 to 17 percent of the weight of the triaryl phosphate ester.
Further, the cleaning agent is one or more of nonanol polyoxyethylene ether, lactone sophorolipid and dirhamnolipid.
Further, the dispersant is one or more of toluene, xylene, trimethylbenzene and ethylbenzene.
Further, the defoaming agent is one or more of tributyl phosphate, polyether modified silicone oil and methyl silicone oil.
Further, the protective agent is one or more of hindered phenol, aromatic amine and phosphite ester.
Further, the hindered phenol is 2, 6-di-tert-butyl-p-cresol.
Further, the aromatic amine is an oxidative coupling product of 4,4' -dioctyldiphenylamine and alkylated N-phenyl- α -naphthylamine.
The preparation method of the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system comprises the following steps:
mixing a dispersant with triaryl phosphate to obtain a base solution; and adding the cleaning agent into the basic solution, stirring uniformly, adding the defoaming agent, stirring to be clear, adding the protective agent, and stirring to be clear to obtain the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system.
Compared with the prior art, the invention has the following beneficial effects:
the composite cleaning agent is an oil-soluble nonpolar cleaning agent, and because triaryl phosphate ester is used as a substrate, the composite cleaning agent can effectively dissolve and thoroughly clean degraded oil in a fire-resistant oil system and oil sludge and aging products in the system by the principle of 'similarity and intermiscibility', and overcomes the problems of residual cleaning agent, pollution to a new oil and oil system, flushing replacement by using a large amount of fire-resistant oil and the like caused by a cleaning method adopting a water-soluble polar chemical cleaning agent. Meanwhile, the dispersing agent, the cleaning agent, the defoaming agent and the protective agent are added, the dispersing agent can enable the cleaning agent and the defoaming agent to be more uniformly dispersed on a substrate, when the dispersing agent, the cleaning agent and the defoaming agent exist simultaneously, a synergistic effect can be generated through interaction, the oil sludge cleaning effect of an oil system is increased, the defoaming function is enhanced, the protective agent can improve the stability of the composite cleaning agent, and the improvement of the stability of the cleaning agent is an important guarantee that qualified oil products can be directly injected into a unit after cleaning and emptying. When the composite cleaning agent is used for cleaning the fire-resistant oil system, the cleaning effect is good, the steps of water cleaning and fire-resistant oil replacement of the fire-resistant oil system are not needed, and the fire-resistant oil system is prevented from being polluted by water and water-soluble chemical substances. After cleaning, only the cleaning agent in the system needs to be emptied, and qualified fire-resistant oil can be directly supplemented to enter an operation state, so that adverse effects on the operating fire-resistant oil can be avoided, and meanwhile, the foam of the fire-resistant oil can be reduced, the oxidation stability is improved, and the deterioration resistance is enhanced.
Drawings
FIG. 1 is a picture of an oil system cooler tube bundle prior to cleaning;
fig. 2 is a photograph of the oil system cooler tube bundle after cleaning.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are provided for purposes of illustration and not limitation.
The invention relates to a composite cleaning agent for cleaning a phosphate fire-resistant oil system, which comprises a substrate and an additive;
wherein the substrate is triaryl phosphate; the additive is a mixture of a cleaning agent, a dispersing agent, a defoaming agent and a protective agent;
the dosage of the cleaning agent is 5-16% of the total weight of the triaryl phosphate and the dispersing agent, the dosage of the defoaming agent is 0.5-1.6% of the total weight of the triaryl phosphate and the dispersing agent, and the dosage of the protective agent is 11-31% of the total weight of the triaryl phosphate and the dispersing agent. The dosage of the dispersant is 6 to 17 percent of that of the triaryl phosphate.
The cleaning agent is one or more of nonanol polyoxyethylene ether, lactone type sophorolipid and dirhamnolipid
The dispersing agent is one or more of toluene, xylene, trimethylbenzene and ethylbenzene.
The defoaming agent is one or more of tributyl phosphate, polyether modified silicone oil and methyl silicone oil.
The protective agent is one or more of hindered phenol, aromatic amine and phosphite ester. The hindered phenol is 2, 6-di-tert-butyl-p-cresol; the aromatic amine is the oxidative coupling product of 4,4' -dioctyldiphenylamine and alkylated N-phenyl-alpha-naphthylamine.
The preparation method of the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system comprises the following steps:
step 1: preparing a base solution from a substrate and a dispersing agent accounting for 6-17% of the substrate by weight, and stirring the base solution at the temperature of 30-45 ℃ under a closed condition for 0.5-1 hour;
step 2: adding a cleaning agent accounting for 5-16% of the weight of the basic solution into the basic solution prepared in the step (1), and stirring for more than 1 hour at the temperature of 30-45 ℃;
and 3, step 3: slowly adding a defoaming agent accounting for 0.5-1.6% of the basic solution into the solution prepared in the step 2 under the condition of stirring at the rotating speed of more than 1000r/min, and continuously stirring at the rotating speed of 3000r/min at the temperature of 30-45 ℃ for more than 3 hours until the solution is transparent and is not turbid;
and 4, step 4: and (3) slowly adding a protective agent accounting for 11-31% of the weight of the basic solution into the solution prepared in the step (2) under the condition of stirring at a rotating speed of more than 1000r/min, and continuously stirring at a rotating speed of 3000r/min at 30-45 ℃ for more than 3 hours until the solution is transparent and not turbid, thus obtaining the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system.
Example 1
1) 7000g of triaryl phosphate, 350g of toluene and 350g of xylene are mixed and heated and stirred in a water bath at 40 ℃ for 1 hour at a rotation speed of 1000r/min to prepare a basic solution.
2) Adding 500g lactonic sophorolipid, 100g rhamnolipid and 100g nonylphenol polyoxyethylene ether into the base solution, and heating and stirring the mixture in water bath at 40 ℃ at the rotating speed of 1000r/min for 1 hour;
3) Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 30g of tributyl phosphate and 30g of polyether modified silicone oil (a manufacturer is a new material Co., ltd., good and much in Dongguan city) into the solution prepared in the step 2, and continuously stirring at the rotating speed of 3000r/min at 45 ℃ for 3 hours until the solution is transparent and is not turbid;
4) 700g of an oxidative coupling product of 2, 6-di-tert-butyl-p-cresol, 200g of 4,4' -dioctyldiphenylamine and alkylated N-phenyl-alpha-naphthylamine were stirred at 1000r/min (manufacturer: vanderbilt, inc., the company's product code is: vanlube 9317) and 400g of phosphite ester are added into the solution prepared in the step 3, and the stirring is continued for 1h at the rotating speed of 1000r/min at the temperature of 40 ℃ until the solution is transparent and not turbid, so that the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is obtained.
The use method of the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system comprises the following steps:
estimating the weight of the fire-resistant oil in an oil system of a certain company, and obtaining the composite cleaning agent for cleaning the phosphate fire-resistant oil system by the following steps: the weight ratio of the fire-resistant oil is 1:100 percent of the cleaning agent is added into an anti-fuel oil system, after the oil system is circularly flushed for 24 hours, the oil system is emptied, and the mixed solution of the composite cleaning agent and the anti-fuel oil is put into an oil tank to be treated.
Referring to fig. 1 and 2, the appearance of the oil cooler in the oil system before and after cleaning can be seen, and the cleaning agent can clean impurities and has a good cleaning effect.
6) Qualified oil products are injected into the fire-resistant oil system and enter a to-be-operated state.
7) And (3) respectively sampling the initial state of the qualified fire-resistant oil after the fire-resistant oil is injected into a fire-resistant oil system and operates for 2 months and 6 months, and detecting the acid value, the resistivity, the foam characteristic (by adopting a GB/T12579-2002 test) and the oil sludge precipitation, wherein the detection results are shown in a table 1.
TABLE 1 oil quality test results for different periods of supplementing qualified oil
As can be seen from Table 1, the cleaning agent of the present invention is shown to have no effect on the subsequent operation of the fuel system.
Example 2
1) 7000g triaryl phosphate and 600g trimethylbenzene in 40 ℃ water bath at 1000r/min speed heating stirring for 1 hours, to prepare the base solution.
2) Adding 600g lactone sophorolipid into the base solution, and heating and stirring at the rotating speed of 1000r/min in water bath at 40 ℃ for 1 hour;
3) Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 30g of tributyl phosphate and 30g of methyl silicone oil into the solution prepared in the step 2, and continuously stirring for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ until the solution is transparent and is not turbid;
4) Under the condition of stirring at the rotating speed of 1000r/min, 600g of 2, 6-di-tert-butyl-p-cresol and 300g of phosphite ester are added into the solution prepared in the step 3, and the solution is continuously stirred at the rotating speed of 1000r/min at the temperature of 40 ℃ for 1h until the solution is transparent and not turbid, so that the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is obtained.
Example 3
1) 7000g of triaryl phosphate, 600g of trimethylbenzene and 100g of ethylbenzene were heated and stirred in a water bath at 40 ℃ for 1 hour at a rotation speed of 1000r/min to prepare a base solution.
2) Adding 400g lactonic sophorolipid and 100g rhamnolipid into the base solution, and heating and stirring in 40 deg.C water bath at 1000r/min for 1 hr;
3) Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 60g of polyether modified silicone oil into the solution prepared in the step 2, and continuously stirring for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ until the solution is transparent and is not turbid;
4) Under the condition of stirring at the rotating speed of 1000r/min, 1100g of 2, 6-di-tert-butyl-p-cresol is added into the solution prepared in the step 3, and the solution is continuously stirred at the rotating speed of 1000r/min at the temperature of 40 ℃ for 1h until the solution is transparent and is not turbid, so that the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is obtained.
Example 4
1) 5008g of triaryl phosphate and 800g of trimethylbenzene are heated and stirred in a water bath at 40 ℃ for 1 hour at the rotating speed of 1000r/min to prepare a base solution.
2) 871.2g lactonic sophorolipid is added into the basic solution and heated and stirred in a water bath at 40 ℃ for 1 hour at the rotating speed of 1000 r/min;
3) Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 80g of polyether modified silicone oil into the solution prepared in the step 2, and continuously stirring for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ until the solution is transparent and is not turbid;
4) And (3) under the condition of stirring at the rotating speed of 1000r/min, adding 1400g of 2, 6-di-tert-butyl-p-cresol into the solution prepared in the step (3), and continuously stirring at the rotating speed of 1000r/min at the temperature of 40 ℃ for 1h until the solution is transparent and is not turbid, thus obtaining the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system.
Example 5
1) 15900g of triaryl phosphate and 1200g of trimethylbenzene are heated and stirred in a water bath at 40 ℃ for 1 hour at the rotating speed of 1000r/min to prepare a basic solution;
2) Adding 1710g lactonic sophorolipid into the basic solution, and heating and stirring for 1 hour in water bath at 40 ℃ at the rotating speed of 1000 r/min;
3) Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 100g of tributyl phosphate into the solution prepared in the step 2, and continuously stirring for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ until the solution is transparent and is not turbid;
4) Under the condition of stirring at the rotating speed of 1000r/min, 2000g of phosphite ester is added into the solution prepared in the step 3, and the solution is continuously stirred at the rotating speed of 1000r/min at the temperature of 40 ℃ for 1h until the solution is transparent and is not turbid, so that the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is obtained.
Example 6
1) 6000g of triaryl phosphate and 360g of toluene are mixed and heated and stirred in a water bath at 40 ℃ for 1 hour at the rotating speed of 1000r/min to prepare a basic solution.
2) Adding 1017.6g lactonic sophorolipid into the basic solution, and heating and stirring the mixture for 1 hour in a water bath at the temperature of 40 ℃ at the rotating speed of 1000 r/min;
3) Under the condition of stirring at the rotating speed of 1000r/min, 31.8g of tributyl phosphate is slowly added into the solution prepared in the step 2, and the stirring is continued for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ until the solution is transparent and is not turbid;
4) Under the condition of stirring at the rotating speed of 1000r/min, 1971.6g of 2, 6-di-tert-butyl-p-cresol is added into the solution prepared in the step 3, and the solution is continuously stirred at the rotating speed of 1000r/min at the temperature of 40 ℃ for 1h until the solution is transparent and is not turbid, so that the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is obtained.
Example 7
1) 6000g of triaryl phosphate and 1020g of toluene are mixed and heated and stirred in a water bath at 40 ℃ for 1 hour at the rotating speed of 1000r/min to prepare a basic solution.
2) Adding 351g lactonic sophorolipid into the basic solution, and heating and stirring for 1 hour at the rotating speed of 1000r/min in water bath at the temperature of 40 ℃;
3) Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 112.32g of tributyl phosphate into the solution prepared in the step 2, and continuously stirring for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ until the solution is transparent and is not turbid;
4) Under the condition of stirring at the rotating speed of 1000r/min, 772.2g of 2, 6-di-tert-butyl-p-cresol is added into the solution prepared in the step 3, and the solution is continuously stirred at the rotating speed of 1000r/min at the temperature of 40 ℃ for 1 hour until the solution is transparent and is not turbid, so that the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is obtained.
The following are comparative experiments on cleaning effect:
respectively taking 5 parts of phosphate fire-resistant oil, wherein each part is 50g.
Directly adding 4g of lactone sophorolipid and 1g of nonanol polyoxyethylene ether into the first phosphate fire-resistant oil, heating and stirring for 1 hour in a water bath at 40 ℃ at the rotating speed of 1000r/min to obtain a sample, wherein the number of the sample is 1-1. The sample was free of dispersants, defoamers, and protectants.
Adding 5g of a mixture of xylene and trimethylbenzene (the volume ratio of xylene to trimethylbenzene is 3. Samples, numbered 1-2, were obtained which had no protectant and no defoamer added.
5g of a mixture of xylene and trimethylbenzene (the volume ratio of xylene to trimethylbenzene is 1). Then 3g of lactone type sophorolipid and 2g of nonanol polyoxyethylene ether are added, and the mixture is heated and stirred for 1 hour in a water bath at the temperature of 40 ℃ at the rotating speed of 1000 r/min. Then slowly adding 0.1g of tributyl phosphate and 0.4g of polyether modified silicone oil under the condition of stirring at the rotating speed of 1000r/min, and continuously stirring for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃ to obtain a sample, wherein the number of the sample is 1-3. The sample was not protected.
5g of a mixture of xylene and trimethylbenzene (the volume ratio of xylene to trimethylbenzene is 3. Then 3g of lactone type sophorolipid, 1g of dirhamnolipid and 1g of nonanol polyoxyethylene ether are added. The mixture was heated and stirred in a water bath at 40 ℃ for 1 hour at a speed of 1000 r/min. Under the condition of stirring at the rotating speed of 1000r/min, slowly adding 0.1g of tributyl phosphate and 0.4g of polyether modified silicone oil, and continuously stirring at the rotating speed of 3000r/min at the temperature of 45 ℃ for 3 hours to obtain a sample, wherein the sample is numbered as 1-4, and the sample is not added with a protective agent.
5g of a mixture of xylene and trimethylbenzene (the volume ratio of xylene to trimethylbenzene is 3. Then 3g of lactone type sophorolipid, 1g of dirhamnolipid and 1g of nonanol polyoxyethylene ether are added. The mixture was heated and stirred in a water bath at 40 ℃ for 1 hour at a speed of 1000 r/min. Then under the condition of stirring at the rotating speed of 1000r/min, 0.1g of tributyl phosphate and 0.4g of polyether modified silicone oil are slowly added, and the stirring is continued for 3 hours at the rotating speed of 3000r/min at the temperature of 45 ℃. Finally, 8g of 2, 6-di-tert-butyl-p-cresol and 3g of phosphite ester are added, and the mixture is continuously stirred for 1h at the rotating speed of 1000r/min at the temperature of 40 ℃ to obtain a sample, wherein the number of the sample is 1-5.
Standing the five samples at room temperature for 24 hours after the preparation of the five samples is finished, wherein the 1-1 sample can observe that the cleaning agent is unevenly dispersed in the fire-resistant oil, and part of the cleaning agent is coagulated; no similar phenomenon was observed for the other samples, indicating that the dispersion could not be achieved without the addition of a dispersant.
Respectively diluting 1-2 samples, 1-3 samples, 1-4 samples and 1-5 samples by 100 times with phosphate fire-resistant oil, and continuously stirring at the rotating speed of 1000r/min at 40 ℃ for 1h to obtain diluted solutions for detecting the cleaning effect and the stability of each sample, wherein the specific process comprises the following steps:
for the filter element which is taken out from the oil system and contains oil sludge pollution, 4 metal sheets are cut out, and the area of the 4 metal sheets is approximate (the area of the 4 metal sheets is about 5 cm) 2 ) And the degree of the pollutants on the surfaces of the 4 metal sheets is close. The 4 metal sheets were numbered 2, 3, 4 and 5, respectively, and after washing the 4 metal sheets with petroleum ether to remove the attached fire resistant oil, the 4 metal sheets were naturally dried for 0.5h, then weighed, respectively, and the weight of each metal sheet before washing was recorded, and the results are shown in table 2.
Respectively putting the No. 2, no. 3, no. 4 and No. 5 metal sheets into the diluted solutions of the 1-2 sample, the 1-3 sample, the 1-4 sample and the 1-5 sample, wherein the volume of the solution is 100mL, continuously stirring at the rotating speed of 300r/min for 3h at 40 ℃, taking out the metal sheets, washing the fire-resistant oil attached to the surfaces of the metal sheets by using petroleum ether, naturally drying for 0.5h, respectively weighing, and recording the weight of the cleaned metal sheets, wherein the results are shown in Table 2.
TABLE 2 comparison of cleaning Effect
As can be seen from Table 2, the larger the weight reduction of the metal piece, the larger the amount of the removed impurities, and the better the cleaning effect.
The following are comparative experiments on stability before and after addition of protective agent:
the hydrolysis stability and oxidation stability of the solutions obtained after dilution of the samples 1 to 4 and 1 to 5 were examined, and the results are shown in Table 3.
TABLE 3 hydrolysis stability and Oxidation stability results
| Sample name | Oxidation stability/(mgKOH/g) | Hydrolytic stability/(mgKOH/g) |
| 1-4 | 0.191 | 1.060 |
| 1-5 | 0.103 | 0.362 |
As can be seen from Table 3, the oxidation stability and hydrolysis stability of the composite cleaning agent with the protective agent are superior to those of the composite cleaning agent without the protective agent, so that the composite cleaning agent prepared by the invention has better stability, does not need to be replaced after being used, and does not cause rapid deterioration of oil products.
Claims (9)
1. The composite cleaning agent for cleaning the phosphate ester fire-resistant oil system is characterized by comprising triaryl phosphate ester, a cleaning agent, a dispersing agent, a defoaming agent and a protective agent; wherein, the dosage of the cleaning agent is 5 to 16 percent of the total weight of the triaryl phosphate and the dispersant, the dosage of the defoaming agent is 0.5 to 1.6 percent of the total weight of the triaryl phosphate and the dispersant, and the dosage of the protective agent is 11 to 31 percent of the total weight of the triaryl phosphate and the dispersant.
2. The compound cleaning agent for cleaning a phosphate ester fire-resistant oil system as claimed in claim 1, wherein the amount of the dispersant is 6-17% of the weight of the triaryl phosphate ester.
3. The composite cleaning agent for cleaning a phosphate ester fire-resistant oil system, according to claim 1, is one or more of nonanol polyoxyethylene ether, lactone sophorolipid and dirhamnolipid.
4. The compound cleaning agent for cleaning a phosphate ester fire-resistant oil system according to claim 1, wherein the dispersing agent is one or more of toluene, xylene, trimethylbenzene and ethylbenzene.
5. The compound cleaning agent for cleaning a phosphate ester fire-resistant oil system according to claim 1, wherein the defoaming agent is one or more of tributyl phosphate, polyether modified silicone oil and methyl silicone oil.
6. The composite cleaning agent for cleaning a phosphate ester fire-resistant oil system according to claim 1, wherein the protective agent is one or more of hindered phenol, aromatic amine and phosphite ester.
7. The compound cleaning agent for cleaning a phosphate ester fire-resistant oil system according to claim 6, wherein the hindered phenol is 2, 6-di-tert-butyl-p-cresol.
8. The composite cleaning agent for cleaning a phosphate ester fire-resistant oil system as claimed in claim 6, wherein the aromatic amine is an oxidative coupling product of 4,4' -dioctyl diphenylamine and alkylated N-phenyl-alpha-naphthylamine.
9. The preparation method of the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system as claimed in any one of claims 1 to 8, characterized by comprising the following steps:
mixing a dispersant with triaryl phosphate to obtain a base solution; and adding the cleaning agent into the basic solution, uniformly stirring, adding the defoaming agent, stirring until the solution is clear, adding the protective agent, and stirring until the solution is clear to obtain the composite cleaning agent for cleaning the phosphate ester fire-resistant oil system.
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