CN107384537A - A kind of vegetable insulating oil and preparation method thereof - Google Patents
A kind of vegetable insulating oil and preparation method thereof Download PDFInfo
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- CN107384537A CN107384537A CN201710510698.5A CN201710510698A CN107384537A CN 107384537 A CN107384537 A CN 107384537A CN 201710510698 A CN201710510698 A CN 201710510698A CN 107384537 A CN107384537 A CN 107384537A
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/082—Inorganic acids or salts thereof containing nitrogen
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/08—Aldehydes; Ketones
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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- C10M2207/24—Epoxidised acids; Ester derivatives thereof
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C10N2010/02—Groups 1 or 11
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/02—Pour-point; Viscosity index
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- 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
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/14—Electric or magnetic purposes
- C10N2040/16—Dielectric; Insulating oil or insulators
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Abstract
The invention belongs to liquid insulating material preparing technical field, and in particular to a kind of vegetable insulating oil and preparation method thereof.The present invention is from cocoanut active charcoal as adsorbent, pass through mechanical ball mill after salpeter solution oxidation processes, to reduce the viscosity of vegetable oil, catalyst is then used as using strontium borate, the alcohol lipid material in maleic anhydride and vegetable oil is set to carry out esterification reaction at high temperature, reduce the freezing point in vegetable oil, glyceryl tristearate is used as crystalline catalysts simultaneously, the impurity of high-solidification point is removed under low-temperature condition, further reduce the freezing point of vegetable insulating oil, it is evaporated under reduced pressure again with mixed alkali liquor, distillation residue is finally collected to mix with antioxidant, it can be prepared by vegetable insulating oil, gained insulating oil of the invention has flash-point height, condensation point is low, the characteristics of viscosity is low, insulating oil items excellent electric properties simultaneously, it is a kind of preferable liquid insulating material.
Description
Technical field
The invention belongs to liquid insulating material preparing technical field, and in particular to a kind of vegetable insulating oil and its preparation side
Method.
Background technology
Insulating oil is a kind of important liquid insulating material, is mainly used in various reactors, transformer, oil-immersed type power and becomes
In the power equipments such as depressor, by impregnating and filling the air gap in abatement apparatus, play a part of improving insulation electrical intensity, together
When can improve the heat dispersion of equipment, have direct influence to the safe operation of power system.
Most popular insulating oil is mineral insulating oil in various countries' power equipment at present.Mineral insulating oil mainly by
Natural oil refining forms.The electric insulating quality and cooling performance of mineral insulating oil are good, and cost is not also high, therefore in oil immersion
There is the applicating history of more than 100 years in insulating power equipment.But with the raising to the various performance requirements of insulating oil, mineral insulation
Also there are many shortcomings in oil, such as：Flash-point is relatively low, fire protecting performance is poor, biodegradability is poor, pollutes the environment during leakage, can not
Regeneration etc..
Under the situation of petroleum resources worsening shortages, a kind of green is developed, the novel insulating oil of environmental protection is paid close attention to as everybody
Focus.Wherein, vegetable insulating oil has good electric property, and flash-point is higher than 300 DEG C, and biological degradation rate is up to 97%, meets
The requirement of electrical equipment fire protecting performance, it is the good environment-friendly liquid dielectric of alternative ore insulating oil.At present, for plant
The research of insulating oil has been achieved for certain progress, and some products are applied in transformer, but still
There are some problems to have to be solved.
Patent No. CN101538500A discloses a kind of insulating oil preparation method using vegetable oil as raw material, the insulating oil with
The vegetable oil such as soybean oil, rapeseed oil, olive oil are raw material, by removing water, hydrogenating, deep refining with deacidification, decompression distillation in alkali
Etc. step, it is eventually adding antioxidant and matal deactivator is made.The insulating oil is obtained by vegetable oil by concise completely, is free of
Noxious material, do not pollute the environment, and can be rapidly and thoroughly biodegradable, meet green requirement.And should
Insulating oil has preferable electric property, and burning-point flash-point is a kind of anti-flammability insulating oil more than 300 DEG C.But the insulation
The complex treatment process of oil, long preparation period, and the problem of viscosity is high, condensation point is high be present, limit its application prospect.
Patent No. CN102222537A discloses a kind of vegetable insulating oil for transformer and preparation method thereof, the invention
By the optimization to the composition of auxiliary material, dosage and refinery practice, the preparation method in patent No. CN101538500A is carried out
Improve.The preparation method that the patent provides is short reaction time, and loss is few, and effect is good, more operational, but does not solve still
Certainly the problem of the viscosity height and high condensation point of refining vegetable oil.
In view of this, it is necessary to research and develop the plant insulation that a kind of modest viscosity, condensation point are low and preparation technology is easy, the cycle is short
Oil product, to solve the above problems.
The content of the invention
The technical problems to be solved by the invention：The problem of viscosity is high, condensation point is high be present for existing vegetable insulating oil,
A kind of and the defects of preparation technology complexity, there is provided vegetable insulating oil and preparation method thereof.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
The vegetable insulating oil of the present invention, includes the raw materials of following parts by weight, 84~86 parts of vegetable oil, 4~8 parts of additives, 2~
3 parts of antioxidants.
The vegetable oil is any one in soybean oil, rapeseed oil, corn oil.
The antioxidant is any one in Tea Polyphenols, gingerol, carnosol.
The preparation of the additive, comprises the following steps：
A. take cocoanut active charcoal, salpeter solution and neopelex to be put into container, stir, heat, while hot mistake
Filter, filter residue is collected, dried, collect dried object；
B. dried object is well mixed with stearic acid, carries out ball milling, ball milling thing is collected, by ball milling thing, glyceryl tristearate, horse
Carry out acid anhydrides and strontium borate stirs, collect stirring mixture, you can obtain additive.
The mass ratio of the cocoanut active charcoal, salpeter solution and neopelex is 4:9:1.
The dried object is 6 with stearic acid mass ratio:1, ball milling thing, glyceryl tristearate, maleic anhydride and strontium borate
Mass ratio be 4~6:3:12~19:1.2~1.5.
A kind of preparation method of vegetable insulating oil, including following preparation process：
（1）Raw material is taken according to parts by weight proportioning；
（2）Vegetable oil and additive are put into container, container is carried out to be heated to 100~105 DEG C, stirring, is cooled to room temperature,
Container is placed at -4~-2 DEG C again and stood, then filtering, collects filtrate；
（3）Filtrate is neutralized using mixed alkali liquor, places into distilling apparatus and is evaporated under reduced pressure, collects distillation residue, then
Distillation residue is stirred with antioxidant, you can obtain vegetable insulating oil.
The mixed alkali liquor is the sodium hydroxide solution of mass fraction 20% and the ammoniacal liquor in mass ratio 5 of mass fraction 25%:3
Mix, the addition of mixed alkali liquor is the 0.8~1.3% of filtrate quality.
The condition of the vacuum distillation is：Pressure is 2.4~3.2kPa, and temperature is 96~98 DEG C, and the time is 1~3h.
Compared with other method, advantageous effects are the present invention：
（1）The cocoanut active charcoal of the invention selected hole prosperity, absorption property good and easily regenerated is molten by nitric acid as adsorbent
Liquid oxidation is handled, while improves its surface-active using surfactant, reuses mechanical ball mill, and further increase activity, is carried
High absorption capacity, and then increase the absorption to the colloid in vegetable oil, to reduce the viscosity of vegetable oil, while utilize coconut activated
The easy reproducibility of charcoal, avoid non-renewable adsorbent and endangered to caused by environment；
（2）The present invention at high temperature enters the alcohol lipid material in maleic anhydride and vegetable oil by the use of strontium borate as catalyst
Row esterification reaction, the freezing point in vegetable oil is reduced, while use glyceryl tristearate as crystalline catalysts, in low temperature shape
The impurity of high-solidification point is removed under state, further reduces the freezing point of vegetable insulating oil；
（3）The present invention can be degradable from natural, good with vegetable insulating oil compatibility, improves vegetable insulating oil
Inoxidizability, the pollution to environment is avoided, while from oil based on the big soybean oil of yield, rapeseed oil, corn oil, reduced
Cost.
Embodiment
The preparation of additive：
A. in mass ratio 4:9:1, cocoanut active charcoal, salpeter solution and neopelex are put into container, with 300r/
Min stirs 20~25min, then container is carried out to be heated to 55~60 DEG C, is incubated 3~5h, filters while hot, collect filter residue, uses
Water washing filter residue is distilled to neutrality, then filter residue is put into 90 DEG C of baking ovens and dries 3~5h, collects dried object；
B. it is 6 in mass ratio:1, dried object is well mixed with stearic acid, is put into ball mill, adds dried object quality 6~9
Times a diameter of 50mm steel ball, with 500r/min 25~30min of ball milling, collect ball milling thing, in mass ratio 4~6:3:12~
19:1.2~1.5, ball milling thing, glyceryl tristearate, maleic anhydride and strontium borate are put into mixer, stirred with 120r/min
10~15min is mixed, collects stirring mixture, you can obtain additive.
Vegetable insulating oil of the present invention includes the raw material of following parts by weight, 84~86 parts of vegetable oil, 4~8 parts of additives, and 2
~3 parts of antioxidants.Vegetable oil is any one in soybean oil, rapeseed oil, corn oil（Vegetable oil is that common vegetable oil passes through
Alkali refining, decolouring, deodorization, the product of dewater treatment）, antioxidant is any one in Tea Polyphenols, gingerol, carnosol.
The preparation of mixed alkali liquor：By the sodium hydroxide solution that mass fraction is 20% and the ammoniacal liquor that mass fraction is 25% by matter
Measure ratio 5:3 mixing, you can.
The preparation method of vegetable insulating oil of the present invention, including following preparation process：
（1）Raw material is taken according to parts by weight proportioning；
（2）Vegetable oil and additive are put into container, container is carried out to be heated to 100~105 DEG C, 4 are stirred with 200r/min
~5h, room temperature is naturally cooled to, then container is placed in 2~3h of standing at -4~-2 DEG C, then filtering, collect filtrate；
（3）Mixed alkali liquor is added in filtrate, the addition of mixed alkali liquor is the 0.8~1.3% of filtrate quality, places into distillation
It is evaporated under reduced pressure in device, sets pressure as 2.4~3.2kPa, temperature is 96~98 DEG C, and distillation time is 1~3h, collects distillation
Residue, then distillation residue is stirred with antioxidant, you can obtain vegetable insulating oil.
Example 1
The preparation of additive：
A. in mass ratio 4:9:1, by cocoanut active charcoal（Gongyi City Song Shan filter material activated carbon factory produces）, salpeter solution and dodecane
Base benzene sulfonic acid sodium salt is put into container, and 20min is stirred with 300r/min, then container is carried out to be heated to 55 DEG C, is incubated 3h, while hot mistake
Filter, filter residue is collected, using distillation water washing filter residue to neutrality, then filter residue is put into 90 DEG C of baking ovens and dries 3h, collect dried object；
B. it is 6 in mass ratio:1, dried object is well mixed with stearic acid, is put into ball mill, adds 6 times of dried object quality
A diameter of 50mm steel ball, with 500r/min ball milling 25min, collect ball milling thing, in mass ratio 4:3:12:1.2, by ball milling thing,
Glyceryl tristearate, maleic anhydride and strontium borate are put into mixer, stir 10min with 120r/min, collection is stirred
Thing, you can obtain additive.
Vegetable insulating oil of the present invention includes the raw material of following parts by weight, 84 portions of soybean oils, 4 parts of additives, and 2 parts of tea are more
Phenol.
The preparation of mixed alkali liquor：By the sodium hydroxide solution that mass fraction is 20% and the ammoniacal liquor that mass fraction is 25% by matter
Measure ratio 5:3 mixing, you can.
The preparation method of vegetable insulating oil of the present invention, including following preparation process：
（1）Raw material is taken according to parts by weight proportioning；
（2）Vegetable oil and additive are put into container, container is carried out to be heated to 100 DEG C, 4h is stirred with 200r/min, it is natural
Room temperature is cooled to, then container is placed at -4 DEG C and stands 2h, then filtering, collects filtrate；
（3）Mixed alkali liquor is added in filtrate, the addition of mixed alkali liquor is the 0.8% of filtrate quality, is placed into distilling apparatus
It is evaporated under reduced pressure, sets pressure as 2.4kPa, temperature is 96 DEG C, distillation time 1h, collects distillation residue, then distillation is remaining
Thing stirs with antioxidant, you can obtains vegetable insulating oil.
Example 2
The preparation of additive：
A. in mass ratio 4:9:1, by cocoanut active charcoal（Gongyi City Song Shan filter material activated carbon factory produces）, salpeter solution and dodecane
Base benzene sulfonic acid sodium salt is put into container, and 23min is stirred with 300r/min, then container is carried out to be heated to 58 DEG C, is incubated 4h, while hot mistake
Filter, filter residue is collected, using distillation water washing filter residue to neutrality, then filter residue is put into 90 DEG C of baking ovens and dries 4h, collect dried object；
B. it is 6 in mass ratio:1, dried object is well mixed with stearic acid, is put into ball mill, adds 8 times of dried object quality
A diameter of 50mm steel ball, with 500r/min ball milling 28min, collect ball milling thing, in mass ratio 5:3:15:1.4, by ball milling thing,
Glyceryl tristearate, maleic anhydride and strontium borate are put into mixer, stir 13min with 120r/min, collection is stirred
Thing, you can obtain additive.
Vegetable insulating oil of the present invention includes the raw material of following parts by weight, 85 portions of rapeseed oils, 6 parts of additives, 2 parts of gingerols.
The preparation of mixed alkali liquor：By the sodium hydroxide solution that mass fraction is 20% and the ammoniacal liquor that mass fraction is 25% by matter
Measure ratio 5:3 mixing, you can.
The preparation method of vegetable insulating oil of the present invention, including following preparation process：
（1）Raw material is taken according to parts by weight proportioning；
（2）Vegetable oil and additive are put into container, container is carried out to be heated to 103 DEG C, 4h is stirred with 200r/min, it is natural
Room temperature is cooled to, then container is placed at -3 DEG C and stands 2h, then filtering, collects filtrate；
（3）Mixed alkali liquor is added in filtrate, the addition of mixed alkali liquor is the 1.1% of filtrate quality, is placed into distilling apparatus
It is evaporated under reduced pressure, sets pressure as 2.8kPa, temperature is 97 DEG C, distillation time 2h, collects distillation residue, then distillation is remaining
Thing stirs with antioxidant, you can obtains vegetable insulating oil.
Example 3
The preparation of additive：
A. in mass ratio 4:9:1, by cocoanut active charcoal（Gongyi City Song Shan filter material activated carbon factory produces）, salpeter solution and dodecane
Base benzene sulfonic acid sodium salt is put into container, and 25min is stirred with 300r/min, then container is carried out to be heated to 60 DEG C, is incubated 5h, while hot mistake
Filter, filter residue is collected, using distillation water washing filter residue to neutrality, then filter residue is put into 90 DEG C of baking ovens and dries 5h, collect dried object；
B. it is 6 in mass ratio:1, dried object is well mixed with stearic acid, is put into ball mill, adds 9 times of dried object quality
A diameter of 50mm steel ball, with 500r/min ball milling 30min, collect ball milling thing, in mass ratio 6:3:19:1.5, by ball milling thing,
Glyceryl tristearate, maleic anhydride and strontium borate are put into mixer, stir 15min with 120r/min, collection is stirred
Thing, you can obtain additive.
Vegetable insulating oil of the present invention includes the raw material of following parts by weight, 86 portions of corn oils, 8 parts of additives, 3 parts of Salvia japonicas
Phenol.
The preparation of mixed alkali liquor：By the sodium hydroxide solution that mass fraction is 20% and the ammoniacal liquor that mass fraction is 25% by matter
Measure ratio 5:3 mixing, you can.
The preparation method of vegetable insulating oil of the present invention, including following preparation process：
（1）Raw material is taken according to parts by weight proportioning；
（2）Vegetable oil and additive are put into container, container is carried out to be heated to 105 DEG C, 5h is stirred with 200r/min, it is natural
Room temperature is cooled to, then container is placed at -2 DEG C and stands 3h, then filtering, collects filtrate；
（3）Mixed alkali liquor is added in filtrate, the addition of mixed alkali liquor is the 1.3% of filtrate quality, is placed into distilling apparatus
It is evaporated under reduced pressure, sets pressure as 3.2kPa, temperature is 98 DEG C, distillation time 3h, collects distillation residue, then distillation is remaining
Thing stirs with antioxidant, you can obtains vegetable insulating oil.
Comparative example：The electrical apparatus insulation oil of lubricating oil Co., Ltd of Shenyang City production.
Vegetable insulating oil made from example 1~3 and the electrical apparatus insulation of comparative example oil are subjected to performance detection, its testing result
As shown in table 1：
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Comparative example | The method of inspection |
| 40 DEG C of kinematic viscosity（mm2/s） | 10.6 | 10.1 | 9.8 | 11.2 | GB/T 265 |
| Condensation point（℃） | -23 | -25 | -29 | -14 | GB/T 510 |
| Flash-point（℃） | 325 | 328 | 332 | 319 | GB/T 261 |
| Frequency breakdown voltage（Gap 2.0mm）/kV | 69.4 | 71.6 | 75.7 | 62.8 | GB/T 507 |
| 90 DEG C of specific insulations（Ω·m） | 8.1×1010 | 8.6×1010 | 8.9×1010 | 7.6×1010 | GB/T 5654 |
| 90 DEG C of dielectric dissipation factors（%） | 0.23 | 0.21 | 0.18 | 0.30 | GB/T 2536 |
The characteristics of viscosity is low, condensation point is low and flash-point is high as it can be seen from table 1 vegetable insulating oil produced by the present invention has, simultaneously
Every electric property of vegetable insulating oil is superior to the electrical apparatus insulation oil of comparative example, is a kind of preferable liquid insulating medium.
Claims (9)
- A kind of 1. vegetable insulating oil, it is characterised in that include the raw material of following parts by weight, 84~86 parts of vegetable oil, 4~8 parts Additive, 2~3 parts of antioxidants.
- 2. vegetable insulating oil according to claim 1, it is characterised in that the vegetable oil is soybean oil, rapeseed oil, corn Any one in oil.
- 3. vegetable insulating oil according to claim 1, it is characterised in that the antioxidant is Tea Polyphenols, gingerol, rat-tail Any one in careless phenol.
- 4. vegetable insulating oil according to claim 1, it is characterised in that the preparation of the additive, comprise the following steps：A. take cocoanut active charcoal, salpeter solution and neopelex to be put into container, stir, heat, while hot mistake Filter, filter residue is collected, dried, collect dried object；B. dried object is well mixed with stearic acid, carries out ball milling, ball milling thing is collected, by ball milling thing, glyceryl tristearate, horse Carry out acid anhydrides and strontium borate stirs, collect stirring mixture, you can obtain additive.
- 5. vegetable insulating oil according to claim 4, it is characterised in that the cocoanut active charcoal, salpeter solution and 12 The mass ratio of sodium alkyl benzene sulfonate is 4:9:1.
- 6. vegetable insulating oil according to claim 4, it is characterised in that the dried object is 6 with stearic acid mass ratio:1, Ball milling thing, glyceryl tristearate, the mass ratio of maleic anhydride and strontium borate are 4~6:3:12~19:1.2~1.5.
- 7. a kind of preparation method of vegetable insulating oil as claimed in claim 1, it is characterised in that including following preparation process：（1）Raw material is taken according to parts by weight proportioning；（2）Vegetable oil and additive are put into container, container is carried out to be heated to 100~105 DEG C, stirring, is cooled to room temperature, Container is placed at -4~-2 DEG C again and stood, then filtering, collects filtrate；（3）Filtrate is neutralized using mixed alkali liquor, places into distilling apparatus and is evaporated under reduced pressure, collects distillation residue, then Distillation residue is stirred with antioxidant, you can obtain vegetable insulating oil.
- 8. the preparation method of vegetable insulating oil according to claim 7, it is characterised in that the mixed alkali liquor is quality point The sodium hydroxide solution of number 20% and the ammoniacal liquor in mass ratio 5 of mass fraction 25%:3 mix, and the addition of mixed alkali liquor is The 0.8~1.3% of filtrate quality.
- 9. the preparation method of vegetable insulating oil according to claim 7, it is characterised in that the condition of the vacuum distillation For：Pressure is 2.4~3.2kPa, and temperature is 96~98 DEG C, and the time is 1~3h.
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