CN104557535A - Method for producing pentaerythritol stearate by taking swill-cooked dirty oil as raw material - Google Patents
Method for producing pentaerythritol stearate by taking swill-cooked dirty oil as raw material Download PDFInfo
- Publication number
- CN104557535A CN104557535A CN201510028030.8A CN201510028030A CN104557535A CN 104557535 A CN104557535 A CN 104557535A CN 201510028030 A CN201510028030 A CN 201510028030A CN 104557535 A CN104557535 A CN 104557535A
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- CN
- China
- Prior art keywords
- sewer oil
- stearic acid
- raw material
- swill
- pentaerythritol stearate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
Abstract
The invention discloses a method for producing pentaerythritol stearate by taking swill-cooked dirty oil as a raw material, belonging to the technical field of preparation of chemical products. The method comprises the following steps: preparing to-be-treated swill-cooked dirty oil into a swill-cooked dirty oil pretreatment solution, preparing swill-cooked dirty oil pretreatment liquor, distilling in a distillation tower, transferring the liquor into a fractionating tower for fractionating, thereby obtaining stearic acid; and cooling the stearic acid, adding pentaerythritol and stannous chloride, uniformly stirring, heating and carrying out an esterification reaction. According to the method disclosed by invention, the swill-cooked dirty oil is taken as the raw material, and the traditional stearic acid preparation raw material, namely palm oil is replaced, so that the swill-cooked dirty oil can be fully utilized, and the production cost of the finished pentaerythritol stearate can be greatly reduced.
Description
Technical field
The invention belongs to Chemicals preparing technical field, particularly relating to a kind of take sewer oil as the method for raw material production pentaerythritol stearate.
Background technology
Sewer oil, makes a general reference all kinds of poor quality oils existed in life, as the edible oil of recovery, the frying oil etc. of Reusability.The appearance of sewer oil, not only to environment, also can may also exist sewer oil backflow dining table and cause serious safe diet hidden danger on the one hand on the other hand.In order to eliminate safety and the environmental protection hidden danger of the generation of above-mentioned sewer oil, people attempt and convert sewer oil to safer, useful product.
Pentaerythritol stearate is a kind of hard white high-melting-point wax, and dissolve in ethanol, benzene, its main application is: highly-efficient lubricant, polyvinyl chloride (PVC) stabilizer and be the raw material of softening agent and rubber ingredients.At present, one of raw material preparing pentaerythritol stearate---stearic acid is mainly that raw material is prepared from plam oil, but, because palmitic price remains high always, cause the preparation cost of pentaerythritol stearate to there is too high defect.
Summary of the invention
The invention provides a kind of take sewer oil as the method for raw material production pentaerythritol stearate, sewer oil is made pentaerythritol stearate as raw material by method, thus while the existing sewer oil of solution exists safety and environmental protection potential problem, the preparation cost of pentaerythritol stearate can be effectively reduced again.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
This production method comprises the following steps:
A, remove the solid matter contained in pending sewer oil, be then heated to 70 DEG C ~ 80 DEG C, and filtered by nanometer overclocking vibration film group, obtain sewer oil pretreatment fluid;
B, sewer oil pretreatment fluid obtained for step A is put into agitator, the vitriol oil accounting for described sewer oil pretreatment fluid quality 0.5% ~ 0.8% is added wherein under stirring condition, stir, be heated to 65 DEG C ~ 75 DEG C, constant temperature stirs 8 hours ~ 12 hours, then stratification, gets supernatant liquid, obtains sewer oil pre-treatment clear liquid;
C, sewer oil pre-treatment clear liquid obtained for step B is first put into distillation tower, be 220 DEG C ~ 240 DEG C in temperature, pressure is distill under the condition of 0MPa ~ 0.001MPa; Then transfer in separation column by distilling the product obtained, be 240 DEG C ~ 250 DEG C in temperature, pressure is fractionation under the condition of 0.075MPa ~ 0.085MPa, obtains stearic acid;
D, stearic acid obtained for step C is first cooled to 85 DEG C ~ 95 DEG C, adds tetramethylolmethane and tin protochloride, stir, then be warming up to 150 DEG C ~ 180 DEG C, esterification 2 hours ~ 4 hours; Wherein, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.15 ~ 0.20:0.005 ~ 0.01.
In technique scheme, technical scheme is more specifically: the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.15:0.01.
Further, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.18:0.008.
Further, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.20:0.005.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
1. the present invention adopts sewer oil as main raw material, replaces traditional stearic acid raw materials---and plam oil, not only can make sewer oil be fully utilized, also can the production cost of significantly finished product pentaerythritol stearate.
2. the finished product pentaerythritol stearate yield that obtains of the present invention is high, and purity is high.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.
Embodiment 1
Basis is that the method for raw material production pentaerythritol stearate comprises the following steps with sewer oil:
A, remove the solid matter contained in pending sewer oil, be then heated to 70 DEG C, and filtered by nanometer overclocking vibration film group, obtain sewer oil pretreatment fluid;
B, sewer oil pretreatment fluid obtained for step A is put into agitator, the vitriol oil accounting for described sewer oil pretreatment fluid quality 0.5% is added wherein under stirring condition, stir, be heated to 65 DEG C, constant temperature stirs 12 hours, then stratification, gets supernatant liquid, obtains sewer oil pre-treatment clear liquid;
C, sewer oil pre-treatment clear liquid obtained for step B is first put into distillation tower, be 220 DEG C in temperature, pressure is distill under the condition of 0MPa; Then transfer in separation column by distilling the product obtained, be 240 DEG C in temperature, pressure is fractionation under the condition of 0.075MPa, obtains stearic acid;
D, stearic acid obtained for step C is first cooled to 85 DEG C, adds tetramethylolmethane and tin protochloride, stir, then be warming up to 150 DEG C, esterification 4 hours; Wherein, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.15:0.01.
The finished product pentaerythritol stearate yield that the present embodiment obtains is 75%, and purity is 99.0%.
Embodiment 2
Basis is that the method for raw material production pentaerythritol stearate comprises the following steps with sewer oil:
A, remove the solid matter contained in pending sewer oil, be then heated to 80 DEG C, and filtered by nanometer overclocking vibration film group, obtain sewer oil pretreatment fluid;
B, sewer oil pretreatment fluid obtained for step A is put into agitator, the vitriol oil accounting for described sewer oil pretreatment fluid quality 0.8% is added wherein under stirring condition, stir, be heated to 75 DEG C, constant temperature stirs 8 hours, then stratification, gets supernatant liquid, obtains sewer oil pre-treatment clear liquid;
C, sewer oil pre-treatment clear liquid obtained for step B is first put into distillation tower, be 240 DEG C in temperature, pressure is distill under the condition of 0.001MPa; Then transfer in separation column by distilling the product obtained, be 250 DEG C in temperature, pressure is fractionation under the condition of 0.085MPa, obtains stearic acid;
D, stearic acid obtained for step C is first cooled to 95 DEG C, adds tetramethylolmethane and tin protochloride, stir, then be warming up to 180 DEG C, esterification 2 hours; Wherein, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.18:0.008.
The finished product pentaerythritol stearate yield that the present embodiment obtains is 75.5%, and purity is 99.1%.
Embodiment 3
Basis is that the method for raw material production pentaerythritol stearate comprises the following steps with sewer oil:
A, remove the solid matter contained in pending sewer oil, be then heated to 75 DEG C, and filtered by nanometer overclocking vibration film group, obtain sewer oil pretreatment fluid;
B, sewer oil pretreatment fluid obtained for step A is put into agitator, the vitriol oil accounting for described sewer oil pretreatment fluid quality 0.6% is added wherein under stirring condition, stir, be heated to 70 DEG C, constant temperature stirs 10 hours, then stratification, gets supernatant liquid, obtains sewer oil pre-treatment clear liquid;
C, sewer oil pre-treatment clear liquid obtained for step B is first put into distillation tower, be 230 DEG C in temperature, pressure is distill under the condition of 0MPa; Then transfer in separation column by distilling the product obtained, be 245 DEG C in temperature, pressure is fractionation under the condition of 0.080MPa, obtains stearic acid;
D, stearic acid obtained for step C is first cooled to 90 DEG C, adds tetramethylolmethane and tin protochloride, stir, then be warming up to 160 DEG C, esterification 3 hours; Wherein, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.20:0.005.
The finished product pentaerythritol stearate yield that the present embodiment obtains is 76%, and purity is 99.1%.
Claims (4)
1. be a method for raw material production pentaerythritol stearate with sewer oil, it is characterized in that comprising the following steps:
A, remove the solid matter contained in pending sewer oil, be then heated to 70 DEG C ~ 80 DEG C, and filtered by nanometer overclocking vibration film group, obtain sewer oil pretreatment fluid;
B, sewer oil pretreatment fluid obtained for step A is put into agitator, the vitriol oil accounting for described sewer oil pretreatment fluid quality 0.5% ~ 0.8% is added wherein under stirring condition, stir, be heated to 65 DEG C ~ 75 DEG C, constant temperature stirs 8 hours ~ 12 hours, then stratification, gets supernatant liquid, obtains sewer oil pre-treatment clear liquid;
C, sewer oil pre-treatment clear liquid obtained for step B is first put into distillation tower, be 220 DEG C ~ 240 DEG C in temperature, pressure is distill under the condition of 0MPa ~ 0.001MPa; Then transfer in separation column by distilling the product obtained, be 240 DEG C ~ 250 DEG C in temperature, pressure is fractionation under the condition of 0.075MPa ~ 0.085MPa, obtains stearic acid;
D, stearic acid obtained for step C is first cooled to 85 DEG C ~ 95 DEG C, adds tetramethylolmethane and tin protochloride, stir, then be warming up to 150 DEG C ~ 180 DEG C, esterification 2 hours ~ 4 hours; Wherein, the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.15 ~ 0.20:0.005 ~ 0.01.
2. according to claim 1 take sewer oil as the method for raw material production pentaerythritol stearate, it is characterized in that: the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.15:0.01.
3. according to claim 1 take sewer oil as the method for raw material production pentaerythritol stearate, it is characterized in that: the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.18:0.008.
4. according to claim 1 take sewer oil as the method for raw material production pentaerythritol stearate, it is characterized in that: the mass ratio of described stearic acid, tetramethylolmethane and tin protochloride three is 1:0.20:0.005.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510028030.8A CN104557535A (en) | 2015-01-21 | 2015-01-21 | Method for producing pentaerythritol stearate by taking swill-cooked dirty oil as raw material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510028030.8A CN104557535A (en) | 2015-01-21 | 2015-01-21 | Method for producing pentaerythritol stearate by taking swill-cooked dirty oil as raw material |
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| CN104557535A true CN104557535A (en) | 2015-04-29 |
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| CN201510028030.8A Pending CN104557535A (en) | 2015-01-21 | 2015-01-21 | Method for producing pentaerythritol stearate by taking swill-cooked dirty oil as raw material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736975A (en) * | 2005-08-24 | 2006-02-22 | 张宪明 | Pentaerythritol stearate preparation method |
| CN102876460A (en) * | 2012-10-30 | 2013-01-16 | 王云 | Flotation agent fatty acid prepared from recycled animal/vegetable oil and swill oil and preparation method thereof |
| CN103012138A (en) * | 2012-12-31 | 2013-04-03 | 齐河县齐翔化工有限公司 | Method for preparing pentaerythritol stearate (PETS) by using illegal cooking oil |
-
2015
- 2015-01-21 CN CN201510028030.8A patent/CN104557535A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736975A (en) * | 2005-08-24 | 2006-02-22 | 张宪明 | Pentaerythritol stearate preparation method |
| CN102876460A (en) * | 2012-10-30 | 2013-01-16 | 王云 | Flotation agent fatty acid prepared from recycled animal/vegetable oil and swill oil and preparation method thereof |
| CN103012138A (en) * | 2012-12-31 | 2013-04-03 | 齐河县齐翔化工有限公司 | Method for preparing pentaerythritol stearate (PETS) by using illegal cooking oil |
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Application publication date: 20150429 |