CN104610052A - Method for preparing pentaerythritol stearate from gutter oil serving as raw material - Google Patents
Method for preparing pentaerythritol stearate from gutter oil serving as raw material Download PDFInfo
- Publication number
- CN104610052A CN104610052A CN201510027989.XA CN201510027989A CN104610052A CN 104610052 A CN104610052 A CN 104610052A CN 201510027989 A CN201510027989 A CN 201510027989A CN 104610052 A CN104610052 A CN 104610052A
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- China
- Prior art keywords
- sewer oil
- stearic acid
- raw material
- pentaerythritol stearate
- gutter oil
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- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
-
- 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
Abstract
The invention discloses a method for preparing pentaerythritol stearate from gutter oil serving as a raw material, and belongs to the technical field of chemical product preparation. The method comprises the steps as follows: to-be-treated gutter oil is made into gutter oil treating fluid, the gutter oil treating fluid is hydrolyzed to obtain gutter oil hydrolysate, and then the gutter oil hydrolysate is put into a distillation tower for distillation and transferred into a fractionating tower for fractionation to obtain stearic acid; the stearic acid is cooled, and pentaerythritol and stannous chloride are added, stirred uniformly and then heated to have an esterification reaction. The gutter oil serves as a main raw material and replaces palm oil serving as a traditional raw material for preparing stearic acid, accordingly, the gutter oil can be fully used, and the production cost of the finished pentaerythritol stearate can be substantially reduced.
Description
Technical field
The invention belongs to Chemicals preparing technical field, particularly relating to a kind of take sewer oil as the method that pentaerythritol stearate prepared by raw material.
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 that pentaerythritol stearate prepared by raw material, 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 preparation method comprises the following steps:
A, remove the solid matter contained in pending sewer oil, then 70 DEG C ~ 80 DEG C are heated to, and filtered by nanometer overclocking vibration film group, then the polyacrylamide accounting for described sewer oil pre-treatment clear liquid quality 0.04% ~ 0.5% is added again, stir 10 minutes ~ 15 minutes, obtain sewer oil treatment solution;
B, be 180 DEG C ~ 200 DEG C by sewer oil treatment solution obtained for step A in temperature, pressure is the Water Under solution 4 hours ~ 6 hours of 2.0MPa ~ 2.5MPa, obtains sewer oil hydrolyzate;
C, sewer oil hydrolyzate 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
This method with sewer oil being pentaerythritol stearate prepared by raw material comprises the following steps:
A, remove the solid matter contained in pending sewer oil, then be heated to 70 DEG C, and filtered by nanometer overclocking vibration film group, then add the polyacrylamide accounting for described sewer oil pre-treatment clear liquid quality 0.04% again, stir 15 minutes, obtain sewer oil treatment solution;
B, be 180 DEG C by sewer oil treatment solution obtained for step A in temperature, pressure is the Water Under solution 6 hours of 2.0MPa, obtains sewer oil hydrolyzate;
C, sewer oil hydrolyzate 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 99.1%.
Embodiment 2
This method with sewer oil being pentaerythritol stearate prepared by raw material comprises the following steps:
A, remove the solid matter contained in pending sewer oil, then be heated to 80 DEG C, and filtered by nanometer overclocking vibration film group, then add the polyacrylamide accounting for described sewer oil pre-treatment clear liquid quality 0.5% again, stir 10 minutes, obtain sewer oil treatment solution;
B, be 200 DEG C by sewer oil treatment solution obtained for step A in temperature, pressure is the Water Under solution 4 hours of 2.5MPa, obtains sewer oil hydrolyzate;
C, sewer oil hydrolyzate 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 99.0%.
Embodiment 3
This method with sewer oil being pentaerythritol stearate prepared by raw material comprises the following steps:
A, remove the solid matter contained in pending sewer oil, then be heated to 75 DEG C, and filtered by nanometer overclocking vibration film group, then add the polyacrylamide accounting for described sewer oil pre-treatment clear liquid quality 0.25% again, stir 12 minutes, obtain sewer oil treatment solution;
B, be 190 DEG C by sewer oil treatment solution obtained for step A in temperature, pressure is the Water Under solution 5 hours of 2.2MPa, obtains sewer oil hydrolyzate;
C, sewer oil hydrolyzate 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 99.2%.
Claims (4)
1. be the method that pentaerythritol stearate prepared by raw material with sewer oil, it is characterized in that comprising the following steps:
A, remove the solid matter contained in pending sewer oil, then 70 DEG C ~ 80 DEG C are heated to, and filtered by nanometer overclocking vibration film group, then the polyacrylamide accounting for described sewer oil pre-treatment clear liquid quality 0.04% ~ 0.5% is added again, stir 10 minutes ~ 15 minutes, obtain sewer oil treatment solution;
B, be 180 DEG C ~ 200 DEG C by sewer oil treatment solution obtained for step A in temperature, pressure is the Water Under solution 4 hours ~ 6 hours of 2.0MPa ~ 2.5MPa, obtains sewer oil hydrolyzate;
C, sewer oil hydrolyzate 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 is the method that pentaerythritol stearate prepared by raw material with sewer oil, 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 is the method that pentaerythritol stearate prepared by raw material with sewer oil, 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 is the method that pentaerythritol stearate prepared by raw material with sewer oil, 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 |
|---|---|---|---|
| CN201510027989.XA CN104610052A (en) | 2015-01-21 | 2015-01-21 | Method for preparing pentaerythritol stearate from gutter oil serving as raw material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510027989.XA CN104610052A (en) | 2015-01-21 | 2015-01-21 | Method for preparing pentaerythritol stearate from gutter oil serving 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 |
| CN102140386A (en) * | 2011-01-24 | 2011-08-03 | 青岛福瑞斯生物能源科技开发有限公司 | Method for degumming biodiesel |
| 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 CN201510027989.XA patent/CN104610052A/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 |
| CN102140386A (en) * | 2011-01-24 | 2011-08-03 | 青岛福瑞斯生物能源科技开发有限公司 | Method for degumming biodiesel |
| 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: 20150513 |
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