CN103435468A - Method for producing stearic acid by utilizing cottonseed oil soapstock - Google Patents
Method for producing stearic acid by utilizing cottonseed oil soapstock Download PDFInfo
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Abstract
The invention discloses a method for producing stearic acid by utilizing cottonseed oil foot, which is mainly implemented by performing water washing, impurity removing, acidolysis, hydrolysis, distillation and hydrogenation on the cottonseed oil foot. Compared with the prior art, the method has the advantages that impurities, gossypol and other pigment substances in the waste cottonseed oil foot can be effectively removed, so that the continuity of subsequent processing means can be guaranteed, the defects that a traditional process cannot perform continuous production and the products are dark in color can be overcome, the product yield and quality can be effectively improved, the yield and quality of stearic acid produced by utilizing vegetable oil leftovers in a traditional method can be greatly increased, waste is turned into wealth and environmental pollution can be effectively prevented by utilizing the waste cottonseed oil foot as a raw material.
Description
Technical field
The present invention relates to a kind of cotton oil pin that utilizes and produce stearic method.
Background technology
Stearic acid is a kind of daily-use chemical industry raw material, is mainly the solid fatty acid obtained in driven, Vegetable oil lipoprotein, and main component is that (C18H36O2, wherein also contain part Palmiticacid (C16H32O2) to stearic acid, and a small amount of oleic acid and linolic acid.
Manufacturing at present the stearic acid product both at home and abroad is mainly the method preparation that utilizes paraffin oxidation style and vegetables oil (as soybean oil, peanut oil, cottonseed wet goods) hydrolysis.
Paraffin belongs to petroleum product, belongs to Nonrenewable resources, therefore can be more and more rare, and price also can be more and more higher, and again because of paraffin oxidation style technique more complicated, so cost is very high.
Although it is simple to utilize vegetables oil to prepare stearic acid technique, need to consume a large amount of vegetables oil, the output of current domestic vegetables oil can't meet domestic needs, needs a large amount of imports every year.
Domestic cotton growing area, all produce a large amount of cottonseeds every year at present, and except part is used for doing seed use, the overwhelming majority is used for squeezing grease.Owing to extracting oil in raw material and technologic singularity with cottonseed, the cotton oil pin produced after oil expression is very many.
The at present utilization for the cotton oil pin generally has following several: one, using its as raw material of manufacturing soap in order to manufacture soap or analogous products.Two, cotton oil distillation residues, after supplementing saponification, is resolved into to lipid acid, then as industrial chemicals, sell relevant producer.The aforesaid method added value is all very low.The source mill of some small scales acts as a fuel the cotton oil pin to burn, and this has caused very large waste from resource view, and What is more, the cotton oil pin toppled over as waste, not only causes waste and contaminate environment.
Summary of the invention
The purpose of this invention is to provide a kind of cotton oil pin that utilizes and produce stearic method.
Purpose of the present invention is mainly by being washed the cotton oil pin removal of impurities, acidolysis, hydrolysis, distillation, hydrogenation realization.
Concrete technical process is:
Washing removal of impurities: cotton oil pin raw material is washed, raw material is preferably by pouring into after Grid screen in feed reservoir again, and first coarse filtration goes out large impurity, as cotton seed hulls, plastic cloth etc., precipitation, more than 8 hours, then draws up layered material liquid and enters into water washing tank, adds the water of feed liquid gross weight 4～6% while heating to 50～60 ℃ by feed liquid, water temperature is controlled at 50～60 ℃, wash after 20 minutes, discharge water, further to discharge impurity and the pigment in feed liquid.
Above-mentioned raw materials adopts steel grating by the flase floor of Grid screen, and the sectional dimension of carrying band steel is 30mm * 2mm, and between centers is 15mm, and cross bar width between centers is 30mm, and structural form is pressure lock steel grating, the zinc-plated processing of surface heat, and it is labeled as G302/15/30L.
Above-mentioned washing can be carried out 2～4 times.
Acidolysis: the feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 45～55 ℃, add by 10～20% of feed liquid total amount the sulphuric acid soln that concentration is 15～25%, reaction is more than 3 hours, by 4～6% of feed liquid gross weight, add again the warm water of 45～55 ℃ to be washed draining after 20 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
Hydrolysis: in hydrolysis kettle, press the mixing ratio 1:35 of water and feed liquid～1:45 weight ratio, in the Water Under solution of 210～230 ℃ of temperature, 1.9～3.5Mpa pressure more than 30 minutes.
Mainly contain lipid acid and some neutral grease in oil plant after acidolysis, these neutral grease must just can be converted into lipid acid and glycerine through hydrolysis.
Preferably reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, obtains glycerine solution, then glycerine solution is distilled and obtains raw glycerine.
Distillation: the feed liquid after hydrolysis is carried out underpressure distillation, so that further purification of fatty acids: 200～260 ℃ of temperature, in the situation of the negative pressure of 0.09～0.1Mpa, carry out, mainly contain oleic acid in the feed liquid after distillation, stearic acid and Palmiticacid, residue is mainly pitch.
Hydrogenation: by 0.5～1.5% hydrogenation of feed liquid gross weight, main purpose is that the unsaturated fatty acids pinolenic acid in the feed liquid after distillation is converted into to saturated stearic acid, further to promote the quality of stearic acid product, by 0.3～0.5% of feed liquid gross weight, add the palladium activated carbon as catalyzer, at 180～200 ℃, under the condition of pressure 2～3Mpa, reacted more than 4 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-3～-6 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
Compared with prior art, the present invention has removed the pigment materials such as impurity in the waste cotton oil foot and gossypol at first effectively, make the continuity of following process means be guaranteed, overcome the darker shortcoming of product colour that traditional technology can not be produced continuously and produce, effectively raise product production and quality, than traditional stearic output and the quality of utilizing plant oil leftover production, all improve a lot, and be to utilize the waste cotton oil foot as raw material, not only turn waste into wealth, and can effectively prevent the pollution of the environment.
Embodiment
embodiment 1:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitate 12 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 5% while heating to 50 ℃ by feed liquid, water temperature is controlled at 50 ℃, wash after 20 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, repeat above-mentioned washing 2 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 45 ℃, add by 10% of feed liquid total amount the sulphuric acid soln that concentration is 20%, react 4 hours, by 5% of feed liquid gross weight, add again the warm water of 45 ℃ ℃ to be washed draining after 30 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:35 of water and feed liquid, in the Water Under solution of 210 ℃ of temperature, 2Mpa pressure more than 30 minutes.Hydrolysis time is reclaimed the byproduct glycerine of discharging with water vapour: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is carried out underpressure distillation, so that further purification of fatty acids: 220 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, press 1% hydrogenation of gained feed liquid gross weight, by 0.5% of feed liquid gross weight, add the palladium activated carbon as catalyzer simultaneously, reacted 4 hours under 180 ℃, the condition of pressure 2～3Mpa.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-5 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 2:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitate 24 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 6% while heating to 60 ℃ by feed liquid, water temperature is controlled at 55 ℃, wash after 60 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can repeat to carry out 3 times again.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 55 ℃, add by 20% of feed liquid total amount the sulphuric acid soln that concentration is 15%, react 5 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 40 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:40 of water and feed liquid, the Water Under solution of 230 ℃ of temperature, 3.5Mpa pressure 60 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is carried out underpressure distillation 2360 ℃ of temperature, 0.1Mpa the situation of negative pressure under distilled after, 0.5% hydrogenation by the feed liquid gross weight, main purpose is that the unsaturated fatty acids pinolenic acid in the feed liquid after distillation is converted into to saturated stearic acid, further to promote the quality of stearic acid product, by 0.5% of feed liquid gross weight, add the palladium activated carbon as catalyzer, at 200 ℃, reacted under the condition of pressure 3Mpa 6 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-5 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 3:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitate 24 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 4% while heating to 55 ℃ by feed liquid, water temperature is controlled at 60 ℃, wash after 30 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 2～4 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 50 ℃, add by 15% of feed liquid total amount the sulphuric acid soln that concentration is 15%, reaction is more than 5 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 40 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:45 of water and feed liquid, in the Water Under solution of 220 ℃ of temperature, 3Mpa pressure more than 60 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is carried out underpressure distillation, so that further purification of fatty acids: 250 ℃ of temperature, 0.095Mpa the situation of negative pressure under distilled, 0.5% hydrogenation by distillation gained feed liquid by gross weight, by 0.5% of feed liquid gross weight, add the palladium activated carbon as catalyzer, at 200 ℃, under the condition of pressure 2.5Mpa, reacted 4 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-3 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 4:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitation is more than 48 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 4% while heating to 55 ℃ by feed liquid, water temperature is controlled at 50 ℃, wash after 60 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 2～4 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 55 ℃, add by 20% of feed liquid total amount the sulphuric acid soln that concentration is 20%, reaction is more than 10 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 50 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:40 of water and feed liquid, in the Water Under solution of 215 ℃ of temperature, 2.5Mpa pressure more than 60 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 240 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, 1% hydrogenation by distillation gained feed liquid by gross weight, add the palladium activated carbon as catalyzer by 0.5% of feed liquid gross weight, at 200 ℃, under the condition of pressure 3Mpa, reacted 10 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-4 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 5:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitation is more than 8 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 5% while heating to 50 ℃ by feed liquid, water temperature is controlled at 50 ℃, wash after 60 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 2～4 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 55 ℃, add by 20% of feed liquid total amount the sulphuric acid soln that concentration is 20%, react 5 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 60 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:45 of water and feed liquid, the Water Under solution of 210 ℃ of temperature, 2.5Mpa pressure 30 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 250 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, 0.5～1.5% hydrogenation by distillation gained feed liquid by gross weight, by 0.3～0.5% of feed liquid gross weight, add the palladium activated carbon as catalyzer, at 180～200 ℃, under the condition of pressure 2～3Mpa, reacted 4 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-5 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 6:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitation is more than 12 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 5% while heating to 50 ℃ by feed liquid, water temperature is controlled at 60 ℃, wash after 30 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 3 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 55 ℃, add by 20% of feed liquid total amount the sulphuric acid soln that concentration is 20%, react 10 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 60 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:35 of water and feed liquid, the Water Under solution of 230 ℃ of temperature, 3Mpa pressure 60 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 220 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, 1% hydrogenation by distillation gained feed liquid by gross weight, add the palladium activated carbon as catalyzer by 0.4% of feed liquid gross weight, at 190 ℃, under the condition of pressure 2Mpa, reacted 5 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-6 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 7:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitate 20 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 5% while heating to 50 ℃ by feed liquid, water temperature is controlled at 60 ℃, wash after 30 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 2 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 55 ℃, add by 20% of feed liquid total amount the sulphuric acid soln that concentration is 15%, reaction is more than 3 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 30 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:35 of water and feed liquid, the Water Under solution of 230 ℃ of temperature, 3.5Mpa pressure 60 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 260 ℃ of temperature, 0.095Mpa the situation of negative pressure under distilled, 1.5% hydrogenation by distillation gained feed liquid by gross weight, add the palladium activated carbon as catalyzer by 0.5% of feed liquid gross weight, at 180 ℃, under the condition of pressure 3Mpa, reacted 10 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-6 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 8:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitate 20 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 4～6% while heating to 55 ℃ by feed liquid, water temperature is controlled at 60 ℃, wash after 30 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 3 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 50 ℃, add by 15% of feed liquid total amount the sulphuric acid soln that concentration is 15%, reaction is more than 6 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 40 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:45 of water and feed liquid, the Water Under solution of 230 ℃ of temperature, 3.5Mpa pressure 30 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 260 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, 0.8% hydrogenation by distillation gained feed liquid by gross weight, add the palladium activated carbon as catalyzer by 0.4% of feed liquid gross weight, at 190 ℃, under the condition of pressure 3Mpa, reacted 12 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-5 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 9:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitation is more than 30 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 5% while heating to 50 ℃ by feed liquid, water temperature is controlled at 60 ℃, wash after 60 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 2 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 50 ℃, add by 0% of feed liquid total amount the sulphuric acid soln that concentration is 20%, react 10 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 60 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:40 of water and feed liquid, the Water Under solution of 220 ℃ of temperature, 3Mpa pressure 90 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 250 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, 0.8% hydrogenation by distillation gained feed liquid by gross weight, add the palladium activated carbon as catalyzer by 0.45% of feed liquid gross weight, at 190 ℃, under the condition of pressure 3Mpa, reacted 8 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-4 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
embodiment 10:
By waste cotton oil foot raw material, pour into again in feed reservoir after by Grid screen, first coarse filtration goes out large impurity, as cotton seed hulls, and plastic cloth etc., precipitation is more than 60 hours, then draw up layered material liquid and enter into water washing tank, add the water of feed liquid gross weight 5% while heating to 50 ℃ by feed liquid, water temperature is controlled at 55 ℃, wash after 40 minutes, discharge water, further to discharge impurity and the pigment in feed liquid, above-mentioned washing can be carried out 2 times.
Feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 55 ℃, add by 15% of feed liquid total amount the sulphuric acid soln that concentration is 15%, react 10 hours, by 5% of feed liquid gross weight, add again the warm water of 55 ℃ to be washed draining after 100 minutes afterwards, to remove sodium sulfate and the part residual sulfuric acid generated after pickling.
In hydrolysis kettle, press the weight mixing ratio 1:40 of water and feed liquid, the Water Under solution of 230 ℃ of temperature, 3.5Mpa pressure 60 minutes.
Reclaim the byproduct glycerine of discharging with water vapour in the time of said hydrolyzed: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, and glycerine is evaporated after reaching finite concentration, and distillation obtains raw glycerine.
Feed liquid after hydrolysis is 250 ℃ of temperature, 0.09Mpa the situation of negative pressure under distilled, 1% hydrogenation by distillation gained feed liquid by gross weight, add the palladium activated carbon as catalyzer by 0.5% of feed liquid gross weight, at 200 ℃, under the condition of pressure 3Mpa, reacted 10 hours.
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-5 ℃, freezing squeezing obtains stearic acid of the present invention, then carries out finished product packing.
Claims (3)
1. one kind is utilized the cotton oil pin to produce stearic method, it is characterized in that main process is as follows:
Washing removal of impurities: cotton oil pin raw material, in feed reservoir, is precipitated more than 8 hours, then draw up layered material liquid and enter into water washing tank, the water that adds feed liquid gross weight 4～6% while heating to 50～60 ℃ by feed liquid, water temperature is controlled at 50～60 ℃, after washing 20 minutes, discharges water;
Acidolysis: the feed liquid after washing is squeezed in pickling tank and carried out acidolysis: in the time of 45～55 ℃, add by 10～20% of feed liquid total amount the sulphuric acid soln that concentration is 15～25%, reaction, more than 3 hours, adds the warm water of 45～55 ℃ to be washed draining after 20 minutes by 4～6% of feed liquid gross weight afterwards again;
Hydrolysis: in hydrolysis kettle, press the mixing ratio 1:35～1:45 of water and feed liquid weight, in the Water Under solution of 210～230 ℃ of temperature, 1.9～3.5Mpa pressure more than 30 minutes;
Distillation: 200～260 ℃ of temperature, carry out the water underpressure distillation in the situation of the negative pressure of 0.09～0.1Mpa;
Hydrogenation: 0.5～1.5% hydrogenation by the feed liquid gross weight, by 0.3～0.5% of feed liquid gross weight, add the palladium activated carbon as catalyzer simultaneously, at 180～200 ℃, under the condition of pressure 2～3Mpa, reacted more than 4 hours;
Feed liquid after hydrogenation reaction is completed is carried out cooling, and under-3～-6 ℃, freezing squeezing gets final product.
2. the cotton oil pin that utilizes according to claim 1 is produced stearic method, it is characterized in that described raw material goes out large impurity by the Grid screen coarse filtration.
3. the cotton oil pin that utilizes according to claim 1 and 2 is produced stearic method, reclaim the byproduct glycerine of discharging with water vapour when it is characterized in that described hydrolysis: the steam that will contain glycerine first passes in the water of tank and makes it cooling and dissolve in water, obtain glycerine solution, then glycerine solution is distilled and obtains raw glycerine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669590A (en) * | 2019-09-30 | 2020-01-10 | 郑州远洋油脂工程技术有限公司 | System and method for continuously producing fatty acid by soapstock |
| CN114426474A (en) * | 2021-11-25 | 2022-05-03 | 新疆华雄再生资源科技有限公司 | Preparation method of cottonseed oil and saponin biological stearic acid |
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| CN110669590A (en) * | 2019-09-30 | 2020-01-10 | 郑州远洋油脂工程技术有限公司 | System and method for continuously producing fatty acid by soapstock |
| CN114426474A (en) * | 2021-11-25 | 2022-05-03 | 新疆华雄再生资源科技有限公司 | Preparation method of cottonseed oil and saponin biological stearic acid |
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