CN101412658B - Method for saponification and acidolysis of hydrogenated castor oil by using high concentration acid and alkali - Google Patents
Method for saponification and acidolysis of hydrogenated castor oil by using high concentration acid and alkali Download PDFInfo
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- CN101412658B CN101412658B CN2008101599664A CN200810159966A CN101412658B CN 101412658 B CN101412658 B CN 101412658B CN 2008101599664 A CN2008101599664 A CN 2008101599664A CN 200810159966 A CN200810159966 A CN 200810159966A CN 101412658 B CN101412658 B CN 101412658B
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- Prior art keywords
- saponification
- acid
- boiling water
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- add
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- 238000007127 saponification reaction Methods 0.000 title claims abstract description 37
- 239000002253 acid Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000003513 alkali Substances 0.000 title claims abstract description 17
- 239000004359 castor oil Substances 0.000 title abstract 3
- 235000019438 castor oil Nutrition 0.000 title abstract 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 title abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 58
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 26
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 24
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 238000009835 boiling Methods 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000007921 spray Substances 0.000 claims description 12
- 230000003068 static effect Effects 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000035484 reaction time Effects 0.000 abstract description 4
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 abstract 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention belongs to a technique for producing 12-hydroxy stearic acid, and in particular to a saponification and acid hydrolysis method for hydrogenated castor oil by using high-concentration acid and alkali. The saponification and acid hydrolysis method for the hydrogenated castor oil adopts 48 percent liquid caustic soda to carry out saponification reaction, and adopts sulphuric acid with the concentration of more than or equal to 96 percent to carry out acid hydrolysis reaction. The saponification and acid hydrolysis method has the advantages that the saponification and acid hydrolysis method improves reaction rate, reduces volume of a saponification and acid hydrolysis tank due to small volume of materials, reduces reaction time greatly, improves equipment utilization rate, is convenient to purify products at the same time, improves quality of the products, reduces sewage drainage, reuses recycled materials in production, and improves yield.
Description
Technical field
The invention belongs to the production technology of 12-oxystearic acid, be specially with the saponification acid hydrolysis method of high density soda acid to THIXCIN.
Background technology
The 12-oxystearic acid is to be raw material with the THIXCIN, produces through saponification, acidolysis process, and outward appearance is the white plates solid, is mainly used in to produce high-grade lithium soap grease, also is the critical materials that guarantees lithium saponify.
At present; THIXCIN is carried out the saponification acidolysis to be produced the process method of 12-oxystearic acid to adopt earlier the vitriol oil, dope alkali dilute with water is the technical process of again Viscotrol C being carried out saponification, acidolysis behind 10% sulfuric acid, 10% the liquid caustic soda; The weak point of its existence is: this technical process take artificial many, waste that the water yield is big, plant factor is low, the technological reaction time is long, speed of response is slow, the whole saponification acidolysis time is at least 2 hours; Production efficiency is low, and cost is high.
Summary of the invention
The object of the invention is exactly to provide a kind of with the saponification acid hydrolysis method of high density soda acid to THIXCIN to above-mentioned defective, and this saponification acid hydrolysis method has improved speed of response; And the volume of material is little, has also just reduced the volume of saponification acid hydrolysis tank, greatly reduces the reaction times; Improve plant factor, be convenient to product simultaneously and purify, improved quality product; Reduce quantity of wastewater effluent, and reclaimed materials has been used in production again, improved productive rate.
Technical scheme of the present invention does, adopting concentration is that 48% liquid caustic soda carries out saponification reaction, adopts concentration to carry out acidolysis reaction more than or equal to 96% sulfuric acid.
Detail operations step of the present invention is that input boiling water 2-3 part in the saponification acid hydrolysis tank adds 10.5 parts of THIXCINs then in jar earlier, adds boiling water 3-5 part simultaneously, opens and stirs, and heats simultaneously; Add 1.5 parts of alkali lye (folding 100%) then, the time that adds alkali lye is 5-10 minute, and the temperature in jar is 95 ℃-100 ℃, after adding alkali lye and finishing, continues to stir also heating 8-15 minute, and the saponification process is replenished boiling water 2-3 part, material Ph=6-8; In jar, add 2.4 parts in sulfuric acid (folding 98%) again, proceed to stir, be the complete layering of transparence until profit, stop to add acid, material Ph=3-5 adds acid time 5-10 minute; Stop heating then, close stirring, and on the charge level of still rotation, spray boiling water; Bleed off waste acid water after the static 10-15 of material minute, open again and stir and heating, in jar, add 3-5 part boiling water; Wash, stop to stir, close heating; Continue again to spray 1-2 part boiling water, after the static layering, bleed off lower floor's washing water and obtain the 12-oxystearic acid.
The use magnitude relation of material is 12 parts of THIXCINs, 1.5 parts of alkali lye (folding 100%), (98%) 2.4 part in sulfuric acid.Wherein, the concentration of alkali lye is 48%, and vitriolic concentration is more than or equal to 96%.
Beneficial effect of the present invention does, this saponification acid hydrolysis method has improved speed of response, and the time of whole saponification acidolysis is 40-50 minute; Greatly reduce the reaction times, and the volume of material is little, has also just reduced the volume of saponification acid hydrolysis tank, improved plant factor; Be convenient to product simultaneously and purify, improved quality product, reduced quantity of wastewater effluent, and reclaimed materials is used in production again; Improve productive rate, practice thrift cost, reduced production cost on the whole, under the identical situation of output; PT reduces half the, and artificial and electric energy loss reduces half the, and under the identical situation of hardware devices such as equipment, throughput doubles.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is carried out detailed explanation.
Embodiment 1
In the saponification acid hydrolysis tank, drop into 2 parts of boiling water earlier, in jar, add 10.5 parts of THIXCINs then, add 5 parts of boiling water simultaneously, open and stir, heat simultaneously; Add 1.5 parts of alkali lye (folding 100%) then, the time that adds alkali lye is 10 minutes, and the temperature in jar is 95 ℃, after adding alkali lye and finishing, continues to stir also and heats 15 minutes, and the saponification process is replenished 2 parts of boiling water, material Ph=6-8; In jar, add 2.4 parts in sulfuric acid (folding 98%) again, proceed to stir, be the complete layering of transparence until profit, stop to add acid, material Ph=3-5 adds the 10 minutes time of acid; Stop heating then, close stirring, and on the charge level of still rotation, spray boiling water; Material bleeds off waste acid water after static 10 minutes, opens and stirs and heating, in jar, adds 3 parts of boiling water; Wash, stop to stir, close heating; Continue again to spray 2 parts of boiling water, after the static layering, bleed off lower floor's washing water and obtain the 12-oxystearic acid.
Embodiment 2
In the saponification acid hydrolysis tank, drop into 3 parts of boiling water earlier, in jar, add 10.5 parts of THIXCINs then, add 3 parts of boiling water simultaneously, open and stir, heat simultaneously; Add 1.5 parts of alkali lye (folding 100%) then, the time that adds alkali lye is 5 minutes, and the temperature in jar is 100 ℃, after adding alkali lye and finishing, continues to stir also and heats 8 minutes, and the saponification process is replenished 3 parts of boiling water, material Ph=6-8; In jar, add 2.4 parts in sulfuric acid (folding 98%) again, proceed to stir, be the complete layering of transparence until profit, stop to add acid, material Ph=3-5 adds the 5 minutes time of acid; Stop heating then, close stirring, and on the charge level of still rotation, spray boiling water; Bleed off waste acid water after the static 10-15 of material minute, open again and stir and heating, in jar, add 5 parts of boiling water; Wash, stop to stir, close heating; Continue again to spray 1 part of boiling water, after the static layering, bleed off lower floor's washing water and obtain the 12-oxystearic acid.
Claims (3)
1. with the saponification acid hydrolysis method of high density soda acid, comprise saponification step and acidolysis step, it is characterized in that adopting concentration is that 48% liquid caustic soda carries out saponification reaction, adopt concentration to carry out acidolysis reaction more than or equal to 96% sulfuric acid to THIXCIN; Its detail operations step is that input boiling water 2-3 part in the saponification acid hydrolysis tank adds 10.5 parts of THIXCINs then in jar earlier, adds boiling water 3-5 part simultaneously, opens and stirs, and heats simultaneously; Add alkali lye then, roll over 100%, 1.5 part, the time that adds liquid caustic soda is 5-10 minute, and the temperature in jar is 95 ℃-100 ℃, after adding liquid caustic soda and finishing, continues to stir also heating 8-15 minute, and the saponification process is replenished boiling water 2-3 part, material pH=6-8; In jar, add sulfuric acid again, roll over 98%, 2.4 part, proceed to stir, be the complete layering of transparence until profit, stop to add sulfuric acid, material pH=3-5 adds 5-10 minute sulfuric acid time; Stop heating then, close stirring, and on the charge level of still rotation, spray boiling water; Bleed off waste acid water after the static 10-15 of material minute, open again and stir and heating, in jar, add 3-5 part boiling water; Wash, stop to stir, close heating; Continue again to spray 1-2 part boiling water, after the static layering, bleed off lower floor's washing water and obtain the 12-oxystearic acid.
2. according to claim 1ly it is characterized in that, in the saponification acid hydrolysis tank, drop into 2 parts of boiling water earlier with the saponification acid hydrolysis method of high density soda acid to THIXCIN; In jar, add 10.5 parts of THIXCINs then; Add 5 parts of boiling water simultaneously, open and stir, heat simultaneously; Add alkali lye then, roll over 100%, 1.5 part, the time that adds liquid caustic soda is 10 minutes, and the temperature in jar is 95 ℃, after adding liquid caustic soda and finishing, continues to stir also and heats 15 minutes, and the saponification process is replenished 2 parts of boiling water, material pH=6-8; In jar, add sulfuric acid again, roll over 98%, 2.4 part, proceed to stir, be the complete layering of transparence until profit, stop to add sulfuric acid, material pH=3-5 adds 10 minutes sulfuric acid time; Stop heating then, close stirring, and on the charge level of still rotation, spray boiling water; Material bleeds off waste acid water after static 10 minutes, opens and stirs and heating, in jar, adds 3 parts of boiling water; Wash, stop to stir, close heating; Continue again to spray 2 parts of boiling water, after the static layering, bleed off lower floor's washing water and obtain the 12-oxystearic acid.
3. according to claim 1ly it is characterized in that, in the saponification acid hydrolysis tank, drop into 3 parts of boiling water earlier with the saponification acid hydrolysis method of high density soda acid to THIXCIN; In jar, add 10.5 parts of THIXCINs then; Add 3 parts of boiling water simultaneously, open and stir, heat simultaneously; Add alkali lye then, roll over 100%, 1.5 part, the time that adds liquid caustic soda is 5 minutes, and the temperature in jar is 100 ℃, after adding liquid caustic soda and finishing, continues to stir also and heats 8 minutes, and the saponification process is replenished 3 parts of boiling water, material pH=6-8; In jar, add sulfuric acid again, roll over 98%, 2.4 part, proceed to stir, be the complete layering of transparence until profit, stop to add sulfuric acid, material pH=3-5 adds 5 minutes sulfuric acid time; Stop heating then, close stirring, and on the charge level of still rotation, spray boiling water; Bleed off waste acid water after the static 10-15 of material minute, open again and stir and heating, in jar, add 5 parts of boiling water; Wash, stop to stir, close heating; Continue again to spray 1 part of boiling water, after the static layering, bleed off lower floor's washing water and obtain the 12-oxystearic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101599664A CN101412658B (en) | 2008-11-14 | 2008-11-14 | Method for saponification and acidolysis of hydrogenated castor oil by using high concentration acid and alkali |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101599664A CN101412658B (en) | 2008-11-14 | 2008-11-14 | Method for saponification and acidolysis of hydrogenated castor oil by using high concentration acid and alkali |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101412658A CN101412658A (en) | 2009-04-22 |
| CN101412658B true CN101412658B (en) | 2012-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2008101599664A Expired - Fee Related CN101412658B (en) | 2008-11-14 | 2008-11-14 | Method for saponification and acidolysis of hydrogenated castor oil by using high concentration acid and alkali |
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| CN (1) | CN101412658B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288627B (en) * | 2013-05-22 | 2015-09-09 | 山东天兴生物科技有限公司 | Take hydrogenated castor oil as the method that 12-oxystearic acid prepared by raw material |
| CN110386872A (en) * | 2018-04-16 | 2019-10-29 | 希锐科技(武汉)有限公司 | A kind of refining methd of 12- hydroxy stearic acid or its ester |
| CN111003783A (en) * | 2019-12-30 | 2020-04-14 | 南通新邦化工科技有限公司 | Method for reducing PH value of wastewater in stearate production |
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2008
- 2008-11-14 CN CN2008101599664A patent/CN101412658B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 王恩.一步皂化富氧法制取1-2羟基硬脂酸锂和氧化蓖麻油生产技术..《内蒙古石油化工》.2002,第28卷(第4期),第26页-28页. * |
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| CN101412658A (en) | 2009-04-22 |
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Owner name: SHANDONG TIANXING BIOTECHNOLOGY CO., LTD. Free format text: FORMER NAME: ZOU COUNTY TIANXING CHEMICAL INDUSTRY CO., LTD. |
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Address after: 256209, Shandong County, Binzhou City, Zouping province Zhen Zhen Economic Development Zone Patentee after: SHANDONG TIANXING BIOTECHNOLOGY Co.,Ltd. Address before: 256209, Shandong County, Binzhou City, Zouping province Zhen Zhen Economic Development Zone Patentee before: ZOU COUNTY TIANXING CHEMICAL INDUSTRY Co.,Ltd. |
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Granted publication date: 20120104 |