CN1686997A - Di-potassium (natrium) sebacate and producing technique - Google Patents
Di-potassium (natrium) sebacate and producing technique Download PDFInfo
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- CN1686997A CN1686997A CN 200510056803 CN200510056803A CN1686997A CN 1686997 A CN1686997 A CN 1686997A CN 200510056803 CN200510056803 CN 200510056803 CN 200510056803 A CN200510056803 A CN 200510056803A CN 1686997 A CN1686997 A CN 1686997A
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Abstract
The present invention relates to a chemical product bipotassium (sodium) sebacate and its production method. Its molecular fermula is C10H16O4K2 (C10H16O4Na2), and its production process includes the following steps: respectively adding sebacic acid and potassium (sodium) hydroxide to solvent so as to obtain sebacic acid solution and potassium (sodium) hydroxide solution, mixing two solutions and making them react to obtain the invented bipotassium (sodium) sebacate. Its content can be up to above 98%, it can be extensively used in the rubber, antifreezing liquid, lubricating grease, high-grade cosmetics and washing product industries.
Description
The technical field is as follows: the invention relates to a chemical product and a manufacturing method thereof, in particular to a dipotassium sebacate (sodium sebacate) and a manufacturing process thereof.
Background art: the sebacic acid is a chemical product produced by using castor as a main raw material, and has quite wide application. Theoretical studies have shown that in the process for producing sebacic acid, sebacic acid is present in the mixture in the form of a salt, mainly a sodium salt, and this sebacate should have a better application prospect. However, it is very difficult toobtain sebacate which has industrial application value in the production process of sebacic acid, and the success has not been achieved so far. Therefore, the sebacate products are a blank which is not required by people in the industry.
The invention content is as follows: the invention aims to provide a sebacate product with industrial application value and a manufacturing process thereof.
The above purpose is realized by the following technical scheme: a chemical product of dipotassium sebacate (sodium salt) is researched, and the molecular formula is as follows: c10H16O4K2(C10H16O4Na2) The structural formula is as follows:
the manufacturing process of the dipotassium (sodium) sebacate comprises the following steps: adding sebacic acid and potassium (sodium) hydroxide into solvent respectively to obtain sebacic acid solution and potassium (sodium) hydroxide solution, and mixing the two solutions to react to obtain dipotassium (sodium) sebacate.
The solvent is water, and the method for preparing the solution by using water as the solvent comprises the following steps: putting water and sebacic acid into a proportioning tank according to the weight ratio of 20-25: 9-11, and adjusting the temperature to 18-22 ℃; putting water and potassium hydroxide (sodium) into another material preparing tank according to the weight ratio of 8-12: 8-12, and controlling the temperature to be 75-85 ℃.
The solvent is ethanol, and the method for preparing the solution by taking the ethanol as the solvent comprises the following steps: putting ethanol and sebacic acid into a mixing tank accordingto the weight ratio of 24-36: 8-12, and adjusting the temperature to 18-22 ℃; ethanol and potassium hydroxide (sodium) are put into another batching tank according to the weight ratio of 98-102: 115-125, and the temperature is controlled to be 45-55 ℃.
The mixed reaction process of the two solutions prepared by taking water as a solvent is as follows: preheating a reaction kettle to 190-9: 1 ℃, respectively adding catalysts into a sebacic acid solution tank and a potassium hydroxide solution tank, uniformly adding the sebacic acid solution and the potassium hydroxide solution into the reaction kettle according to the proportion of 7-9: 1, heating to 242-248 ℃ when the temperature of the reaction kettle is reduced to 128-135 ℃, starting a vacuum pump after reacting for 2.5-3.5 hours, reacting for 50-70 minutes in a high vacuum state, maintaining the temperature at 130-136 ℃, starting sampling and testing when the current of the reaction kettle reaches 38-46(A), drying until the current is qualified, and sending the dried product to a finished product tank for packaging when the moisture is less than or equal to 1%.
The mixed reaction process of the two solutions prepared by taking ethanol as a solvent is as follows: preheating a reaction kettle to 85-95 ℃, simultaneously starting circulating water of a condenser to ensure that the water temperature is below 18 ℃, uniformly adding a sebacic acid solution and a potassium hydroxide solution into the reaction kettle according to the proportion of 7-9: 1, then starting an alcohol return valve to slowly raise the temperature to 320-332 ℃, starting sampling and testing after the alcohol return reaction is carried out for 2 hours, starting a vacuum pump to carry out vacuum dealcoholization, cooling and recycling after the samples are qualified, stopping a heat-conducting oil pump when the current of the reaction kettle reaches 38-42(A), entering a drying process when the temperature in the kettle is reduced to 32-38 ℃, and sending the products into a finished product tank to be packaged when the moisture is less than or equal to 1%.
The content of the dipotassium sebacate (sodium sebacate) prepared by the scheme is more than 98 percent, and the dipotassium sebacate (sodium sebacate) can be widely applied to the manufacturing processes of rubber, antifreeze, lubricating grease, high-grade cosmetics, washing products and the like, and has very considerable market prospect.
The implementation mode is as follows:
the first embodiment: water is used as solvent. After four times of water filtration, the tap water is purified by manganese sand and anion-cation resin, distilled and cooled to remove mechanical impurities and iron and chlorine plasma components in the water so as to reach the standard of pure water, and then pumped into a water storage tank for standby.
And (4) sending the sebacic acid into a No. 1 feeding chamber, and checking whether the indoor temperature and humidity meet the requirements.
And (3) sending potassium hydroxide (sodium hydroxide) into a No. 2 feeding chamber, and checking whether the indoor temperature and humidity meet the requirements.
Heating a heat conduction oil furnace to 198 ℃, starting a heat conduction oil pump to circularly preheat the reaction kettle to 195 ℃, then injecting 1.136 tons of pure water into the 1# batching tank, starting a batching stirrer, adding 500 kilograms of sebacic acid at the speed of 1.5 kilograms per second, and adjusting the temperature of the 1# batching tank to 20 ℃. And then 108 kilograms of pure water is injected into the No. 2 batching tank, 108 kilograms of potassium (sodium) hydroxide are added at the speed of 1.5 kilograms persecond, the batching stirrer is started, and the temperature of the batching tank is controlled between 79 ℃ and 81 ℃.
Simultaneously, 1.5 kilograms of ionic nickel catalyst is respectively put into the No. 1 and No. 2 batching tanks, then a reaction kettle stirrer is started, sebacic acid solution and potassium hydroxide solution are uniformly added into the reaction kettle according to the proportion of 8: 1, when the temperature of the reaction kettle is reduced to 131.8 ℃, the temperature is started to rise to 245 ℃, the temperature is controlled to be 244-246 ℃, after 3 hours of reaction, a vacuum pump is started to react for 1 hour in a vacuum state, and the temperature is maintained to be 133.8 ℃. Then the heat-conducting oil pump is stopped, and when the current of the reaction kettle reaches 42(A), the laboratory is informed to sample. After the test is unqualified, relevant reactions are continued or auxiliary materials are added, after the test is qualified, an absorber, a drying tower, a drying fan, a feeder and a material puller are started, the motor frequency of each device is adjusted according to the process requirement, the device reaches the speed required by the process to be dried, the dried material entering the intermediate tank is informed to a laboratory to detect the moisture, and when the moisture is less than or equal to 1%, the material is sent to a finished product tank to be packaged.
The second embodiment: ethanol is used as a solvent. And (4) sending the sebacic acid into a No. 1 feeding chamber, and checking whether the indoor temperature and humidity meet the requirements.
And (3) sending potassium hydroxide (sodium hydroxide) into a No. 2 feeding chamber, and checking whether the indoor temperature and humidity meet the requirements.
When the temperature of the heat-conducting oil furnace is raised to 100 ℃,a heat-conducting oil pump is started to circulate the pre-pyrolysis reaction kettle to enable the temperature to reach 90 ℃, and meanwhile, circulating water of a condenser of the pyrolysis reaction kettle is started to enable the circulating water of the condenser to reach below 18 ℃.
1.5 tons of ethanol are injected into the 1# batching tank, the batching stirrer is switched on, 500 kg of sebacic acid are added at a rate of 3 kg per second, and the temperature of the batching tank is adjusted to 20 ℃. Then 100 kg of ethanol is injected into the No. 2 batching tank, the batching stirrer is started, 120 kg of potassium hydroxide (sodium hydroxide) is added at the speed of 3 kg per second, and the temperature of the batching tank is controlled between 49 ℃ and 51 ℃.
Starting a cracking reaction kettle stirrer, uniformly adding a sebacic acid solution and a potassium hydroxide solution into the reaction kettle according to the proportion of 8: 1, starting an alcohol return valve after all the sebacic acid solution and the potassium hydroxide solution are completely put into the reaction kettle, slowly raising the temperature to 328 ℃, circularly reacting the alcohol return for 2 hours, and then informing a laboratory to sample. And (5) carrying out unqualified test and continuous reaction, starting a vacuum pump after the test is qualified, carrying out vacuum dealcoholization, and cooling and recovering. And (3) when the current of the reaction kettle reaches 40(A), stopping the heat-conducting oil pump, when the temperature in the kettle is reduced to 35 ℃, starting the absorber, the drying tower, the drying fan, the feeder and the material puller, adjusting the motor frequency of each device according to the process requirement to ensure that the device reaches the speed required by the process for drying, informing a laboratory to detect the moisture of the material entering the intermediate tank after drying, and when the moisture is less than or equal to 1%, sending the material into a finished product tank for packaging.
The final reaction process of the above two examples is:
KOOC(CH2)8COOK has a molecular weight of 278.2
NaOOC(CH2)8Molecular weight of COONa is 246
The product appearance is as follows: white, extremely fine powder.
Physical and chemical indexes of double potassium sebacate
| Item | Standard value | Item | Standard value |
| Water content is less than or equal to | 1 | pH value | 7-9 |
| The water insoluble substance content is less than or equal to | 1 | The particle size (120 mesh transmittance%) > or more | 95 |
| Chloride ion (PPm) | 300 | Iron ion (PPm) is less than or equal to | 100 |
| The content is more than or equal to | 98 |
Physicochemical index of disodium sebacate
| Item | Standard value | Item | Standard value |
| Water content is less than or equal to | 1 | pH value | 7-9 |
| The water insoluble substance content is less than or equal to | 1 | Particle size (120 mesh transmittance%)≥ | 95 |
| Chloride ion (PPm) | 300 | ||
| The content is more than or equal to | 98 |
Claims (10)
1. A chemical product of dipotassium sebacate (sodium salt) is characterized in that: the molecular formula of the sebacic acid dipotassium (sodium) salt is as follows: C10H16O4K2(C10H16O4Na2) having the formula:
2. a manufacturing process of a dipotassium (sodium) sebacate is characterized by comprising the following steps: adding sebacic acid and potassium (sodium) hydroxide into solvent respectively to obtain sebacic acid solution and potassium (sodium) hydroxide solution, and mixing the two solutions to react to obtain dipotassium (sodium) sebacate.
3. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the solvent is water, and the method for preparing the solution by using water as the solvent comprises the following steps: putting water and sebacic acid into a proportioning tank according to the weight ratio of 20-25: 9-11, and adjusting the temperature to 18-22 ℃; putting water and potassium hydroxide (sodium) into another batching tank according to the weight ratio of 8-12: 8-12, and controlling the temperature to be 75-85 ℃.
4. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the solvent is ethanol, and the method for preparing the solution by taking the ethanol as the solvent comprises the following steps: putting ethanol and sebacic acid into a mixing tank according to the weight ratio of 24-36: 8-12, and adjusting the temperature to 18-22 ℃; ethanol and potassium hydroxide (sodium) are put into another batching tank according to the weight ratio of 98-102: 115-125, and the temperature is controlled to be 45-55 ℃.
5. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the mixed reaction process of the sebacic acid solution and the potassium hydroxide solution which are prepared by taking water as a solvent comprises the following steps: preheating a reaction kettle to 190-9: 1 ℃, respectively adding catalysts into a sebacic acid solution tank and a potassium hydroxide solution tank, uniformly adding the sebacic acid solution and the potassium hydroxide solution into the reaction kettle according to the proportion of 7-9: 1, heating to 242-248 ℃ when the temperature of the reaction kettle is reduced to 128-135 ℃, starting a vacuum pump after reacting for 2.5-3.5 hours, reacting for 50-70 minutes in a high vacuum state, maintaining the temperature at 130-136 ℃, starting samplingand testing when the current of the reaction kettle reaches 38-46(A), drying until the current is qualified, and sending the dried product to a finished product tank for packaging when the moisture is less than or equal to 1%.
6. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the mixed reaction process of the sebacic acid solution and the potassium hydroxide solution which are prepared by taking ethanol as a solvent comprises the following steps: preheating a reaction kettle to 85-95 ℃, simultaneously starting circulating water of a condenser to ensure that the water temperature is below 18, uniformly adding a sebacic acid solution and a potassium hydroxide solution into the reaction kettle according to the proportion of 7-9: 1, then starting an alcohol return valve to slowly raise the temperature to 320-332 ℃, starting sampling and testing after the alcohol return reaction is carried out for 2 hours, starting a vacuum pump to carry out vacuum dealcoholization, cooling and recycling after the samples are qualified, stopping a heat-conducting oil pump when the current of the reaction kettle reaches 38-42(A), entering a drying process when the temperature in the kettle is reduced to 32-38 ℃, and sending the products into a finished product tank to be packaged when the moisture is less than or equal to 1%.
7. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the method for preparing the solution by using water as a solvent comprises the following steps: putting water and sebacic acid into a mixing tank according to the weight ratio of 1136: 500, and adjusting the temperature to 20 ℃; putting water and potassium hydroxide (sodium) into another mixing tank according to the weight ratio of 1: 1, and controlling the temperature to be79-81 ℃; then the catalyst is respectively put into the two tanks.
8. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the solvent is ethanol, and the method for preparing the solution by taking the ethanol as the solvent comprises the following steps: putting ethanol and sebacic acid into a material mixing tank according to the weight ratio of 3: 1, and adjusting the temperature to 20 ℃; adding ethanol and potassium (sodium) hydroxide at a weight ratio of 100: 120 into another mixing tank, and controlling the temperature at 45-55 deg.C.
9. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the mixed reaction process of the sebacic acid solution and the potassium hydroxide solution which are prepared by taking water as a solvent comprises the following steps: preheating a reaction kettle to 195 ℃, uniformly adding a sebacic acid solution and a potassium hydroxide solution into the reaction kettle according to the proportion of 8: 1, heating to 245 ℃ when the temperature of the reaction kettle is reduced to 131.8 ℃, starting a vacuum pump after 3-hour reaction, reacting for 1 hour in a high vacuum state, maintaining the temperature at 133.8 ℃, starting sampling and testing when the current of the reaction kettle reaches 42(A) is observed, and drying until the current is qualified until the moisture is less than or equal to 1%, and then sending the reaction kettle into a finished product tank for packaging.
10. The process for the manufacture of the dipotassium (sodium) sebacate salt of claim 2, characterized in that: the mixed reaction process of the sebacic acid solution and the potassium hydroxide solution which are prepared by taking ethanol as a solvent comprises the following steps: preheating a reaction kettle to 90 ℃, simultaneously starting circulating water of a condenser to ensure that the water temperature is below 18, uniformly adding a sebacic acid solution and a potassium hydroxide solution into the reaction kettle according to the proportion of 8: 1, then starting an alcohol return valve to slowly raise the temperature to 328 ℃, starting sampling and testing after the alcohol return reaction is carried out for 2 hours, starting a vacuum pump to carry out vacuum dealcoholization, cooling and recycling after the reaction kettle is qualified, stopping a heat-conducting oil pump when the current of the reaction kettle reaches 40(A), entering a drying process when the temperature in the reaction kettle is reduced to 35 ℃, and drying until the moisture is less than or equal to 1% and sending the reaction kettle into a finished product tank to be packaged.
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| CNB200510056803XA CN1324000C (en) | 2005-03-25 | 2005-03-25 | Di-potassium (natrium) sebacate and producing technique |
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| CNB200510056803XA CN1324000C (en) | 2005-03-25 | 2005-03-25 | Di-potassium (natrium) sebacate and producing technique |
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| CN88105680A (en) * | 1988-02-29 | 1988-09-28 | 邵阳市有机化工厂 | Phenol diluent and manufacture method thereof |
| IT1232161B (en) * | 1989-07-31 | 1992-01-25 | Sigma Tau Ind Farmaceuti | USE OF SEBACIC ACID AND ITS DERIVATIVES IN ENTERAL AND PARENTAERAL FEEDING AND PHARMACEUTICAL COMPOSITIONS CONTAINING SUCH COMPOUNDS |
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Owner name: INNER MONGOLIA WEIYU BIOLOGICAL TECHNOLOGY CO., LT Free format text: FORMER OWNER: KANGSITE OIL CHEMICAL CO., LTD., TONGLIAO CITY Effective date: 20140102 |
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Free format text: CORRECT: ADDRESS; FROM: 028000 TONGLIAO, INNER MONGOLIA AUTONOMOUS REGION TO: 028024 TONGLIAO, INNER MONGOLIA AUTONOMOUS REGION |
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Effective date of registration: 20140102 Address after: Horqin district industrial park Plum Street Map Muli north, East Tongliao, the Inner Mongolia Autonomous Region Tongda Road 028024 Patentee after: INNER MONGOLIA WEIYU BIOLOGICAL TECHNOLOGY CO., LTD. Address before: 028000, No. 119, main street, Horqin district, the Inner Mongolia Autonomous Region, Tongliao Patentee before: Kangsite Oil Chemical Co., Ltd., Tongliao City |