CN100339349C - Preparation method of long chain fatty acid calcium salt - Google Patents
Preparation method of long chain fatty acid calcium salt Download PDFInfo
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- CN100339349C CN100339349C CNB2004100830600A CN200410083060A CN100339349C CN 100339349 C CN100339349 C CN 100339349C CN B2004100830600 A CNB2004100830600 A CN B2004100830600A CN 200410083060 A CN200410083060 A CN 200410083060A CN 100339349 C CN100339349 C CN 100339349C
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- saponification
- fatty acid
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- chain fatty
- calcium salt
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Abstract
The present invention discloses a preparation method of long chain fatty acid calcium salt used for additive of high-energy feed. The present invention has the main technical characteristics that natural vegetable fat and NaOH solution are mixed and are saponified for three hours under a condition that the temperature of soap solution is under 95 to 98 DEG C; when a saponification value is not less than 93%, a saponification endpoint reaches, CaCl2 solution is used for precipitation, and the long chain fatty acid calcium salt is obtained by washing, dewatering, drying and pulverizing. The long chain fatty acid calcium salt produced by the present invention is a kind of protective fat, has the advantages of high energy density, good feeding effect, energy supply and calcium supply, is particularly suitable for high yield milk cows of which the weight is excessively reduced caused by that the milk cows are always in energy negative balance during the lactation period, and can also be used in high-energy feed of beef cattle, table poultry, etc. A saponification reaction kettle of the present invention is heated by electric heat-oil bath, environmental protection and high efficiency can be realized, and generalization and application are conveniently realized. The product produced by the method is green nutritional type feed additive and has the advantages of good quality, less consumption, convenient storage and transport and convenient operation.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the long chain fatty acid calcium salt of high energy feed supplement, refer in particular to natural plant grease and substitute the preparation method that animal grease is produced long chain fatty acid calcium salt.
Background technology
In the past, it was raw material production with butter, sheep wet goods animal tallow that China produces long chain fatty acid calcium salt, and all was the mode of production of handicraft workshop.Along with the outburst of mad cow disease, China has forbidden that animal feedstuff adds and uses in ruminating animal.Therefore, substitute animal grease with natural plant grease and produce the requirement that fatty acid calcium meets " green " nutrition type feed additive.Long chain fatty acid calcium salt preparation technology's gordian technique is the fat hydrolysis technology.At present, the method of fat hydrolysis mainly contains following several: 1, decomposition agent method, and this method is simple to operate, installation cost is low, raw oil material is applied widely, but hydrolysis time is long, the consumption quantity of steam is many, the equipment and materials corrosion is big, contain Phenylsulfonic acid in the water lotion, enter the river pollution water source.2, high pressure does not have the catalase continuous hydrolysis process, and this method technology is simple, degree of hydrolysis is high, energy consumption is low, but cost of equipment is big, is not suitable for medium-sized and small enterprises and adopts.3, grease adds enzyme hydrolysis method, this method have power consumption less, low, the percent hydrolysis of installation cost is than advantages such as height, but production cost is very high.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of long chain fatty acid calcium salt, this method is to be that the alternative animal grease of raw material (as rapeseed oil, soya-bean oil, sunflower seed oil, oleum lini, vegetable seed wet goods) prepares fatty acid calcium salt with the crude vegetal, it adopts double decomposition, at normal temperatures and pressures reaction.
Technical problem of the present invention is solved by following scheme: the preparation method of long chain fatty acid calcium salt, it is characterized in that: get crude vegetal and place the saponification reaction still, the tap water that adds 5～9 times of its weight simultaneously, beginning oil bath heating, 110～140 ℃ of oil bath temperatures, getting oil again, to weigh 15%～24% content be that 95% technical grade NaOH is dissolved in the water of 3～5 times of its weight, disposable the joining in the saponification reaction still of NaOH solution begun saponification, mix saponification temperature and remain on 95～98 ℃, after the saponification 3 hours, get a little soap lye every half an hour and survey its saponification value, when saponification value 〉=92%, be the saponification terminal point, soap lye is transferred to the cooling of pulpous state soap storage tank, when the soap lye temperature is reduced to 25～70 ℃, gets oil and weigh 20%～50% anhydrous CaCl
2Be dissolved in the water of 1～3 times of its weight, CaCl
2Solution joins lentamente in the pulpous state soap storage tank and fast and stirs, precipitated in a large number, being deposited in of obtaining carried out thorough washing to pH value in the rinse bath be 7 o'clock, use the oil press press dewatering again, then squeezing is sloughed the product of most water and pulverize, be long chain fatty acid calcium salt in 24～48 hours with 35 ℃～60 ℃ hot gas flow dryings with the sulfuration bed dryer.
Advantage of the present invention is:
1, technology of the present invention is simple, easy to operate, installation cost is low, less energy consumption, good product quality, yield height.
2, the present invention substitutes the turbid fat of animal with various natural plant greases and produces the requirement that fatty acid calcium meets ' green ' nutrition type feed additive.
3, all be to use white lime as the calcium source in the past, though white lime is cheap, speed of response is slow, and the bad control of add-on, and it is more to consume energy, poor product quality.The present invention uses CaCl
2As the calcium source, mainly be because of its solvability is good, Ca
2+Be easy to the Na in the substituted fatty acid sodium
+Generate fatty acid calcium, byproduct sodium-chlor is water-soluble simultaneously easily removes, and CaCl
2Low price.
Boiler Steam heating with the past when 4, saponification reaction still of the present invention designs is improved to electric heating one oil bath heating, so both environmental protection, and the efficient height is convenient to operate and apply again.
5, product of the present invention reduces the ratio of fine fodder in the feed owing to the energy level that effectively raises in the feed, can reduce feed cost, has overcome the shortcoming of neutral grease.Therefore, long chain fatty acid calcium salt is adapted at using in the aquacultures such as milk cow, beef cattle, fryer.And its production cost is lower, usage quantity is few, and storage transports, uses all very easy.So this product has vast market and popularizing application prospect.The long chain fatty acid calcium salt that the present invention produces is present best a kind of protected fat; its energy density height, good feeding effect, complementary energy is replenished the calcium simultaneously, and the high yield cow that particularly causes excess weight to descend to often being in negative energy balance in lactation period is significant.This preparation method is lower to equipment requirements, less investment, be fit to medium-sized and small enterprises and adopt.
Description of drawings
Accompanying drawing is the technological process of production figure of long chain fatty acid calcium salt.
Embodiment
Embodiment 1: takes by weighing rapeseed oil 120Kg and is added in the saponification reaction still, add the 720Kg tap water, and beginning oil bath heating, oil bath temperature is 110～140 ℃.Simultaneously, take by weighing NaOH (technical grade, content 95%) 26.05Kg and be dissolved in the 80Kg water, in the disposable adding reactor of NaOH solution, the beginning saponification, saponification temperature remains on the soap lye temperature between 95～98 ℃.Behind saponification 3h, get a little soap lye every half an hour and survey its saponification value, when saponification value=93.73%, be the saponification terminal point.Soap lye is transferred to the cooling of pulpous state soap storage tank, when the soap lye temperature is reduced to 70 ℃, accurately takes by weighing anhydrous CaCl
2(technical grade) 56.49Kg is dissolved in the 60Kg water, adds CaCl lentamente
2Solution also stirs fast, is precipitated in a large number.To be deposited in that to carry out thorough washing to pH value in the rinse bath be at 7 o'clock, use the oil press press dewatering again, and then squeezing be sloughed the product of most water and pulverize, be long chain fatty acid calcium salt in 48 hours with 50 ℃ of hot gas flows dryings with the sulfuration bed dryer.Then, long chain fatty acid calcium salt being carried out anti-oxidation tech handles.
Embodiment 2: takes by weighing soybean oil 100Kg and is added in the saponification reaction still, add the 840Kg tap water simultaneously, and beginning oil bath heating, oil bath temperature is 110～140 ℃.Simultaneously, take by weighing NaOH (technical grade, content 95%) 18.73Kg and be dissolved in the 60Kg water, in the disposable adding reactor of NaOH solution, the beginning saponification, saponification temperature remains on the soap lye temperature between 95～98 ℃.Behind saponification 3h, get a little soap lye every half an hour and survey its saponification value, when saponification value=94.69%, be the saponification terminal point.Soap lye is transferred to the cooling of pulpous state soap storage tank, when the soap lye temperature is reduced to 50 ℃, accurately takes by weighing anhydrous CaCl
2(technical grade) 23.54Kg is dissolved in the 60Kg water, adds CaCl lentamente
2Solution also stirs fast, is precipitated in a large number.To be deposited in that to carry out thorough washing to pH value in the rinse bath be at 7 o'clock, use the oil press press dewatering again, and then squeezing be sloughed the product of most water and pulverize, be long chain fatty acid calcium salt in 48 hours with 40 ℃ of hot gas flows dryings with the sulfuration bed dryer.Then, long chain fatty acid calcium salt being carried out anti-oxidation tech handles.
Embodiment 3: takes by weighing sunflower seed oil 130Kg and is added in the saponification reaction still, add the 700Kg tap water simultaneously, and beginning oil bath heating, oil bath temperature is 110～140 ℃.Simultaneously, take by weighing NaOH (technical grade, content 95%) 25.58Kg and be dissolved in the 80Kg water, in the disposable adding reactor of NaOH solution, the beginning saponification, saponification temperature remains on the soap lye temperature between 95～98 ℃.Behind saponification 3h, get a little soap lye every half an hour and survey its saponification value, when saponification value=94.31%, be the saponification terminal point.Soap lye is transferred to the cooling of pulpous state soap storage tank, when the soap lye temperature is reduced to 40 ℃, accurately takes by weighing anhydrous CaCl
2(technical grade) 39.17Kg is dissolved in the 100Kg water, adds CaCl lentamente
2Solution also stirs fast, is precipitated in a large number.To be deposited in that to carry out thorough washing to pH value in the rinse bath be at 7 o'clock, use the oil press press dewatering again, and then squeezing be sloughed the product of most water and pulverize, be long chain fatty acid calcium salt in 48 hours with 35 ℃ of hot gas flows dryings with the sulfuration bed dryer.Then, long chain fatty acid calcium salt being carried out anti-oxidation tech handles.
Claims (1)
1, the preparation method of long chain fatty acid calcium salt, it is characterized in that: get crude vegetal and place the saponification reaction still, the tap water that adds 5～9 times of its weight simultaneously, beginning oil bath heating, 110～140 ℃ of oil bath temperatures, getting oil again, to weigh 15%～24% content be that 95% technical grade NaOH is dissolved in the water of 3～5 times of its weight, disposable the joining in the saponification reaction still of NaOH solution begun saponification, mix saponification temperature and remain on 95～98 ℃, after the saponification 3 hours, get a little soap lye every half an hour and survey its saponification value, when saponification value 〉=92%, be the saponification terminal point, soap lye is transferred to the cooling of pulpous state soap storage tank, when the soap lye temperature is reduced to 25～70 ℃, gets oil and weigh 20%～50% anhydrous CaCl
2Be dissolved in the water of 1～3 times of its weight, CaCl
2Solution joins lentamente in the pulpous state soap storage tank and fast and stirs, precipitated in a large number, being deposited in of obtaining carried out thorough washing to pH value in the rinse bath be 7 o'clock, use the oil press press dewatering again, then squeezing is sloughed the product of most water and pulverize, be long chain fatty acid calcium salt in 24～48 hours with 35 ℃～60 ℃ hot gas flow dryings with the sulfuration bed dryer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100830600A CN100339349C (en) | 2004-09-22 | 2004-09-22 | Preparation method of long chain fatty acid calcium salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100830600A CN100339349C (en) | 2004-09-22 | 2004-09-22 | Preparation method of long chain fatty acid calcium salt |
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| CN1752064A CN1752064A (en) | 2006-03-29 |
| CN100339349C true CN100339349C (en) | 2007-09-26 |
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| CNB2004100830600A Expired - Fee Related CN100339349C (en) | 2004-09-22 | 2004-09-22 | Preparation method of long chain fatty acid calcium salt |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337877B (en) * | 2008-08-07 | 2011-05-25 | 中山市华明泰化工材料科技有限公司 | Method for preparing higher fatty acid alkali salt |
| CN103461706B (en) * | 2013-09-02 | 2014-12-10 | 河北省畜牧兽医研究所 | Laying hen feed additive rich in omega-3 fatty acid and using method of feed additive |
| CN103689239A (en) * | 2013-12-23 | 2014-04-02 | 宜兴市天石饲料有限公司 | Preparation method of rumen-through double-layer coated betaine |
| CN105566090B (en) * | 2014-10-13 | 2018-12-11 | 浙江医药股份有限公司新昌制药厂 | A kind of preparation method of polyunsaturated fatty acid calcium |
| CN106278871A (en) * | 2016-08-08 | 2017-01-04 | 苏志刚 | Utilize the method that fatty acid calcium prepared by Oleum Gossypii semen |
| CN108077928A (en) * | 2017-11-30 | 2018-05-29 | 郭英群 | A kind of health products and preparation method thereof |
| CN111264703B (en) * | 2018-12-05 | 2023-05-26 | 丰益(上海)生物技术研发中心有限公司 | Granular fatty acid calcium product and preparation method thereof |
| CN114214372A (en) * | 2021-12-20 | 2022-03-22 | 新疆天药生物科技有限公司 | Method for synthesizing long-chain liquid unsaturated fatty acid calcium salt |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03128342A (en) * | 1989-06-09 | 1991-05-31 | Gumma Pref Gov Kasei Sangyo:Kk | Production of fatty acid calcium salts comprising foots as raw material |
| CN1571328A (en) * | 2003-07-17 | 2005-01-26 | 深圳市中兴通讯股份有限公司 | Super large-scale cross connection device and method used for synchronous digital transmission system |
-
2004
- 2004-09-22 CN CNB2004100830600A patent/CN100339349C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03128342A (en) * | 1989-06-09 | 1991-05-31 | Gumma Pref Gov Kasei Sangyo:Kk | Production of fatty acid calcium salts comprising foots as raw material |
| CN1571328A (en) * | 2003-07-17 | 2005-01-26 | 深圳市中兴通讯股份有限公司 | Super large-scale cross connection device and method used for synchronous digital transmission system |
Non-Patent Citations (3)
| Title |
|---|
| 大豆脂肪酸钙代替油脂饲喂肉仔鸡的试验 王文杰等，饲料研究，第8期 2003 * |
| 脂肪酸钙加工工艺的研究 孙国君等，石河子大学学报（自然科学版），第7卷第1期 2003 * |
| 长链脂肪酸钙的合成及其在奶牛生产中的应用 葛蔚等，中国饲料，第12期 2002 * |
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