CN1256412C - Method for low-pressure continuous hydrolysis preparation of fatty acid - Google Patents
Method for low-pressure continuous hydrolysis preparation of fatty acid Download PDFInfo
- Publication number
- CN1256412C CN1256412C CN 200310118949 CN200310118949A CN1256412C CN 1256412 C CN1256412 C CN 1256412C CN 200310118949 CN200310118949 CN 200310118949 CN 200310118949 A CN200310118949 A CN 200310118949A CN 1256412 C CN1256412 C CN 1256412C
- Authority
- CN
- China
- Prior art keywords
- pressure
- fatty acid
- reactor
- water
- lipid acid
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a method for preparing fatty acid by continuous hydrolyzation at low pressure, which is characterized in that the weight ratio of water to oil is 5 to 30:100, and the pressure at the outlet of a pump is controlled at the range of 0.02 to 0.5Mpa(preferably at the range of 0.1 to 0.4Mpa). Raw materials are under the reaction of heat exchange in a heat exchanger, and then are put into a reactor after being heated in a heating furnace to the temperature of 250 to 500DEGC; reaction products are led out after the raw materials react in the reactor for 2 to 30 minutes, and the reaction products are separated to obtain crude fatty acid and fuel gas or directly distilled to obtain fatty acid. In the method, the temperature conditions of hydrolyzation are changed and the operation pressure is reduced to reduce the pressure grade of total system devices, shorten processing routes, reduce water consumption in the processes, lower the load and the pollution discharge intensity of a water system, omit a glycerol recovery system, lower energy consumption, decrease production cost, shorten reaction time and greatly enhance the productivity of devices.
Description
Technical field
The present invention relates to a kind of low pressure continuous hydrolysis and produce the method for lipid acid, particularly utilize various greases can be under the low pressure condition in the process of producing lipid acid continuous hydrolysis produce the method for lipid acid.
Background technology
Traditional lipid acid production method has several modes such as saponification method, acidization and mesohigh hydrolysis method.Except that high-pressure process, all the other several modes all need to carry out under the effect of catalyzer, remove relatively difficulty of residual catalyzer, the wastewater treatment load greatly, blowdown, pollution treatment intensity height, percent hydrolysis are low, all are lower than 95%.Though the mesohigh hydrolysis method is produced lipid acid without catalyzer, the percent hydrolysis height, but all need the outer high temperature and high pressure steam that supplies in order to satisfy the needed temperature and pressure of hydrolytic process, the middle setting-out condition of separating is: pressure 2.5～3.5Mpa temperature, 230～250 ℃ (seeing CN1074043C); The highly pressured hydrolysis condition is: pressure 5～5.5Mpa, 230～260 ℃ of temperature (see " lipid acid and deep processing handbook thereof), the reaction times, the acid number of gained lipid acid was generally 180mgKOH/g all greater than 3 hours.
The reason that the mesohigh method can not be widelyd popularize is that the huge investment that forms of the high-pressure system of production equipment and too high process cost make that medium-sized and small enterprises are unable to be born, and causes the lipid acid production cost high.
Summary of the invention
The objective of the invention is to overcome the prior art deficiency, provide a kind of low pressure continuous hydrolysis to produce the method for lipid acid, by changing the temperature condition of hydrolysis, reduce working pressure, and then the pressure rating of reduction total system equipment, shorten operational path, reduce facility investment significantly, shorten the reaction times, increase substantially plant capacity.
Detailed method step of the present invention is: with raw material (various greases, acidifying wet goods) and water, through measuring by pump delivery, water weight of oil ratio is 5～30: 100, pump discharge pressure is controlled in 0.02～0.5Mpa scope, be preferably between 0.1～0.4Mpa, enter after the heat exchange of raw material process interchanger and enter reactor after process furnace is heated between 250～500 ℃, in reactor, react after 2～30 minutes and draw reaction product, get croude fatty acids and fuel gas or straight run distillation after the separation and obtain lipid acid.
Can regulate water-oil ratio, temperature of reaction, reaction pressure, reaction times according to the different material oil product among the present invention; Raw material mixes with water, homogenization degree high more help more the reaction.Fuel gas enters process furnace can do the fuel use, and croude fatty acids also can get lipid acid and residue after distillation.Distillation promptly can be that air distillation also can be underpressure distillation.
The reaction product of drawing from reactor promptly can be through entering separator after the water cooler cooling, separate croude fatty acids and fuel gas, croude fatty acids also can get lipid acid and residue after distillation, also can directly enter fractionating system without cooling, obtains fuel gas, lipid acid, residue respectively.
The present invention is by improving hydrolysis temperature, make it under the very high temperature of reaction of grease or acidifying oil, to be hydrolyzed, make the by-product glycerol cracking under this temperature, do not produce glycerine and produce fuel gas, broken reacting phase balance in the former technology, make to be reflected under the low pressure condition and can to carry out, and greatly shortened the reaction times, improved percent hydrolysis; Owing to reduced the oil gas dividing potential drop, discharging continuous still battery has continuously also changed the distillation pattern that must use underpressure distillation in the past, and the process simplification energy consumption is reduced.
Major technique characteristics of the present invention are:
The first, grease or the acidifying wet goods raw material of producing lipid acid all can be hydrolyzed not adding under catalyzer, the constant-pressure and high-temperature condition, and hydrolysis pressure is less than 0.4Mpa, and temperature is between 250～500 ℃.Compare with the high temperature middle-pressure process with high temperature and high pressure method, reduced the pressure rating of working pressure and device, deducted high pressure steam system simultaneously and significantly reduced the investment amount, improved the safety coefficient of producing.
The second, hydrolysis is to carry out continuously, and the reaction times is short, and the reaction times only needs 2～30 minutes (raw material difference, reaction times difference), has improved the throughput of device, has improved returns of investment.
Three, removed the glycerine recovery system, do not produced glycerine and produce fuel gas, though the glycerine price is higher than fuel gas, calculated its production cost and overall income, the latter is much larger than the former.Do not reclaim glycerine, shortened technical process, simplified schedule of operation, reduced process cost.The fuel gas that produces can satisfy the demand for fuel of production process, and it is suitable that income that fuel produces and glycerine reclaim the benefit that produces.
Four, reduced process water, water consumption can be controlled in inlet amount 30% within, process water can be recycled, and has deducted sewage disposal load and sewage discharge intensity.
Five, reaction product can obtain croude fatty acids and fuel gas after cooling, also can directly enter Distallation systm and distill, and obtains lipid acid.
The present invention shortens operational path owing to not using high pressure steam to remove high pressure steam system, reduces the process water amount, reduces water system load and blowdown intensity; Remove the glycerine recovery system, the minimizing productive expense cuts down the consumption of energy; Shorten the reaction times, increase substantially plant capacity.
Description of drawings
Fig. 1 is a kind of process flow diagram that low pressure continuous hydrolysis of the present invention is produced lipid acid.Among the figure: the 1-feedstock pump, the 2-water pump, the 3-interchanger, the 4-water cooler, 5-divides flow container, 6-process furnace, 7-reactor 8-fuel gas outlet pipe, 9-croude fatty acids outlet pipe, 10-by-product and water outlet pipe.
Embodiment
Embodiment 1:
Use technical process shown in Figure 1, on the small-sized continuous hydrolysis device of 20 kilograms/hour of processing poweies, the acidifying oil that will after acidification, obtain by cottonseed oil foot, its acid number is that 68mgKOH/g and water measure through volume pump, and water-oil ratio is 1: 4, pump discharge pressure 0.4Mpa, enter and enter reactor after tubular oven is heated between 380 ℃, react 6 minutes, after separating, get croude fatty acids and fuel gas after water cooler enters separator after being chilled to normal temperature.Croude fatty acids gets lipid acid after distillation, its acid number is: 193mgKOH/g, 32 ℃ at zero pour.
Embodiment 2:
Be raw material with Oleum Gossypii semen (food grade) on the device of embodiment 1, operational condition is: water-oil ratio 28: 100, and pump discharge pressure 0.36Mpa, 395 ℃ of temperature of reaction, the reaction times is 15 minutes, the distillation of cooling back, obtaining the lipid acid acid number is 190.5mgKOH/g.
Embodiment 3:
On the device of embodiment 1, use the raw material of embodiment 1, the reaction product that reaction conditions obtains, but directly enter fractionating system, can obtain fuel gas from the top without cooling, the bottom obtains residue, obtains lipid acid from the middle part, and its acid number is 196.5mgKOH/g, 33 ℃ at zero pour, color and luster is qualified.
Claims (4)
1. a low pressure continuous hydrolysis is produced the method for lipid acid, with grease or acidifying oil is that raw material heats the reaction that is hydrolyzed, its characteristics are raw material and water, through measuring by pump delivery, water weight of oil ratio is 5～30: 100, pump discharge pressure is controlled in 0.02～0.5Mpa scope, after the heat exchange of raw material process interchanger, entering process furnace is heated to 250～500 ℃ and enters reactor, in reactor, react after 2～30 minutes and draw reaction product, get croude fatty acids and fuel gas or straight run distillation after the refrigerated separation and obtain lipid acid.
2. method according to claim 1 is characterized in that pump discharge pressure is controlled between 0.1～0.4Mpa.
3. method according to claim 1 is characterized in that the reaction product of drawing from reactor enters separator after the supercooler cooling, separate croude fatty acids and fuel gas, croude fatty acids obtains lipid acid after distillation.
4. according to claim 1 or 3 described methods, it is characterized in that the distillation mode is air distillation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310118949 CN1256412C (en) | 2003-11-27 | 2003-11-27 | Method for low-pressure continuous hydrolysis preparation of fatty acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310118949 CN1256412C (en) | 2003-11-27 | 2003-11-27 | Method for low-pressure continuous hydrolysis preparation of fatty acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1544595A CN1544595A (en) | 2004-11-10 |
| CN1256412C true CN1256412C (en) | 2006-05-17 |
Family
ID=34338082
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310118949 Expired - Fee Related CN1256412C (en) | 2003-11-27 | 2003-11-27 | Method for low-pressure continuous hydrolysis preparation of fatty acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1256412C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304545C (en) * | 2005-05-16 | 2007-03-14 | 浙江大学 | Method for preparing fatty acid through continuous hydrolyzing grease without catalysis in near critical aqueous medium |
| CN100398633C (en) * | 2006-05-19 | 2008-07-02 | 浙江大学 | Method for non-catalytic lanolin hydrolyzed preparation of lanolin acid and lanolin alcohol using in near critical water medium |
| CN110499216A (en) * | 2019-08-29 | 2019-11-26 | 安徽省瑞芬得油脂深加工有限公司 | The linoleic preparation method of high-purity |
| CN111171963A (en) * | 2020-02-25 | 2020-05-19 | 珠海天汇能源科技有限公司 | Grease hydrolysis device and grease hydrolysis method |
-
2003
- 2003-11-27 CN CN 200310118949 patent/CN1256412C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1544595A (en) | 2004-11-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105384639B (en) | Refined purifying plant for continuously producing LITHIUM BATTERY dimethyl carbonate | |
| CN1076687A (en) | The C of continuous production higher fatty acid 1-4The method of alkyl ester | |
| EP1944285A1 (en) | Method and apparatus for preparing fatty acid esters with alcohol recycling | |
| CN103451027B (en) | Esterification method for preparing biodiesel using waste oils and fats | |
| CN105586154A (en) | Continuous esterification method for preparing biodiesel from waste grease | |
| CN1256412C (en) | Method for low-pressure continuous hydrolysis preparation of fatty acid | |
| CN103242966A (en) | Technology process for producing biodiesel and key preparation device | |
| CN108479653B (en) | Integral microchannels reaction unit and the method for preparing two-(2- chloroethyl) di-phosphate esters using the device | |
| CN102586027A (en) | Continuous production method of biodiesel from waste oil/fat | |
| CN106929163B (en) | Acid reducing system for waste oil | |
| CN107311864A (en) | A kind of chemical purification process | |
| CN1053691C (en) | Hydrogenation technology | |
| CN210012834U (en) | Continuous esterification production device for waste oil | |
| CN110357771A (en) | A kind of partition tower process of methyl lactate hydrolysis rectifying | |
| CN103242896A (en) | Reduced pressure distillation method with low energy consumption and deep total distillation rate | |
| CN1664087A (en) | Process for producing monomeric fatty acid | |
| CN1294243C (en) | Super critical CO2 precision separating process device | |
| CN219540248U (en) | Propionyl chloride production system | |
| CN203807408U (en) | Full-automatic controlled environment-friendly catalytic cracking integrated refining device for waste mineral oil | |
| CN211471311U (en) | Fine fractionation device for hydrogenation process | |
| CN221051802U (en) | Diesel oil separation device of wax oil hydrogenation system | |
| CN114805027B (en) | Process and device for producing higher fatty alcohol by continuous rectification | |
| CN212067783U (en) | Biodiesel byproduct crude glycerine continuous dealcoholization device | |
| CN215288650U (en) | Fractionating system | |
| CN210656811U (en) | Fractionating system in diesel oil and naphtha production process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060517 Termination date: 20151127 |