CN1071911A - The preparation method of stearate - Google Patents
The preparation method of stearate Download PDFInfo
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- CN1071911A CN1071911A CN 91109875 CN91109875A CN1071911A CN 1071911 A CN1071911 A CN 1071911A CN 91109875 CN91109875 CN 91109875 CN 91109875 A CN91109875 A CN 91109875A CN 1071911 A CN1071911 A CN 1071911A
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- stearate
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- stearic acid
- oxide
- oxyhydroxide
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Abstract
Stearate preparation method provided by the invention is that to adopt metal oxide or oxyhydroxide and stearic acid be to be heated to 103～130 ℃ in the medium to stir saponification reaction and directly produce stearate at water.Utilize the inventive method can produce stearate such as barium, lead, zinc, cadmium.Its advantage is not have inorganic salt in the stearate, and technical process is short, low equipment investment, and the yield height, it is low to consume energy, and no waste liquid produces, and is free from environmental pollution.Utilize the inventive method also can produce other higher fatty acid such as cetylate or naphthenate.
Description
The present invention relates to metal ion in a kind of stearate molecule is insoluble in the stearate of water when existing with oxide compound, oxyhydroxide form preparation method.
The stearate that present industrial preparation calcium stearate, barium, zinc, lead, its metal oxide of this class of cadmium, oxyhydroxide are insoluble in water all adopts double decomposition, at first stearic acid and sodium oxide reaction are generated sodium stearate during preparation, and then utilize sodium stearate and the respective metal water soluble salt produced to carry out replacement(metathesis)reaction, thereby finally make desired stearate.The advantage of double decomposition is to react easily to carry out, and technological operation is easily grasped.But, need to consume a large amount of sodium hydroxide in the technology, and being finally converted into sodium salt, these sodium bleed off with waste liquid, therefore employed sodium hydroxide also just wastes, next is to contain a large amount of inorganic salt in the stearate that is generated by metathesis, consuming a large amount of hot water washs, water content height in the stearate after the washing, hear rate is big when dehydrating, moreover, produce a large amount of brine waste discharging backs in the production process environment is produced pollution, especially produce plumbous, the waste water of discharging in the stearate processes such as cadmium not only contains a large amount of inorganic salts but also contains human body, the lead of biological toxic effect, cadmium ion.Owing to a large amount of sodium hydroxide high energy consumption of double decomposition consumption, long flow process, cause stearate manufacturing cost height.Long flow path, equipment is many, and the tooling device investment is big.
It is short to the purpose of this invention is to provide a kind of flow process, energy consumption is low, less investment, no waste liquid generation, environmentally safe, do not contain other inorganic salt in the finished product, produce the preparation method who is insoluble in the stearate of water when metal ion exists with oxide compound or oxyhydroxide in the stearate molecule by metal oxide or oxyhydroxide and stearic acid direct reaction.
Adopt metal oxide, oxyhydroxide and stearic acid direct reaction are produced stearate, be that the employing fineness is the metal oxide or the oxyhydroxide meal of 200 order screen underflows, to be reaction medium with water put into WATER AS FLOW MEDIUM with metal oxide or oxyhydroxide and stearic acid is heated with stirring to 103～120 ℃ and react in confined conditions, make metal oxide or hydroxide solids particle suspension in WATER AS FLOW MEDIUM and with metal oxide or oxyhydroxide, mix to contact and carry out saponification reaction generation stearate, its reaction times is 60～230 minutes, and the medium water yield is metal oxide or oxyhydroxide+stearic acid (weight): water (weight) is 1: 7～10.Reaction is finished the afterreaction resultant and is carried out centrifugation, and the gained filter also is particulate state or coccoid, carries out drying again after wet product are pulverized and is the finished product stearate.The effect capable of circulation of isolated drainage is used.
When the method for utilizing metal oxide or oxyhydroxide to produce stearate is produced calcium stearate, carrying out permanent calculation of material by reaction equation determines, per two mol stearic acid add 1 mol calcium oxide or calcium hydroxide determines to throw metering, with fineness is that (or the stearic acid of calcium hydroxide and charging capacity is put into calcium oxide+stearic acid (weight): water weight is 1: 8～10 water to 200 order all-pass powdery calcium oxide, airtight heating in reactor, under constantly stirring, in 103～107 ℃ and stir, under heating and agitation condition, reacted 50～70 minutes.Reaction is finished after-filtration and is told filter cake, and drainage returns use, carries out drying after filter and the pulverizing and is the finished product calcium stearate.
When utilizing metal oxide or oxyhydroxide and stearic acid direct reaction to produce Zinic stearas, determine charging capacity by permanent calculation of reaction equation, promptly 2 mol stearic acid add 1 mol zinc oxide, with fineness is that the powdery zinc oxide of 200 mesh sieve all-pass and the stearic acid of charging capacity are put into stearic acid ten zinc oxide (weight): water (weight) is 1: 7～9 water, airtight stirring heating was reacted 200～230 minutes under 106～108 ℃ of conditions in reactor, the reaction after-filtration that finishes is told filter also, after filter cake is pulverized again drying be the finished product Zinic stearas.
When utilizing metal oxide or oxyhydroxide and stearic acid direct reaction to produce barium stearate by reaction equation carry out material permanent calculate determine, every mol stearic acid adds 1 mol hydrated barta, with fineness is that the powdery hydrated barta of 200 mesh sieve all-pass and the stearic acid of charging capacity are put into stearic acid decahydro barium oxide (weight): water (weight) is 1: 7～9 water, airtight stirring heating was reacted 60～80 minutes under 103～105 ℃ of conditions in reactor, filter after reaction finishes and tell filter also, carry out drying after filter and the pulverizing and be the finished product barium stearate.(annotating: when using hydrated barta eight water things, do not need 200 order all-pass).
When utilizing metal oxide or oxyhydroxide and stearic reaction directly to produce lead stearate, carry out perseverance by reaction equation and calculate definite charging capacity, per 2 mol stearic acid add 1 mol plumbous oxide, with the fineness of charging capacity is that the powdery plumbous oxide of all-pass under 200 mesh sieves and the stearic acid of charging capacity and charging capacity are put into stearic acid ten plumbous oxide (weight): water (weight) is 1: 8～10 water, airtight stirring heating in reactor, in temperature is stirring reaction 200～230 minutes under 110～120 ℃ of conditions, after finishing, reaction filters, carry out drying after filter and the pulverizing and be the finished product lead stearate, drainage returns use.
Utilize the reaction of metal oxide or oxyhydroxide and stearic acid directly to produce cadmium stearate, add 1 mol Cadmium oxide by the per 2 mol stearic acid of the permanent calculation of reaction equation and determine charging capacity.With the fineness of charging capacity is that the powdery Cadmium oxide of 200 order all-pass and the stearic acid of charging capacity are put into stearic acid ten Cadmium oxides (weight): water (weight) is 1: 8～10 water, airtight stirring heating in reactor was reacted 200～230 minutes under 110～120 ℃ of conditions.Filter after reaction finishes, the wet product of filter cake are pulverized after drying and are the cadmium stearate finished product, and drainage can be recycled.
Utilize the reaction of employing metal oxide provided by the invention or oxyhydroxide and stearic acid directly to produce stearate.Technical process is short, and the equipment consumption is few, invests little.No waste liquid produces, and has eliminated the pollution to environment, has saved a large amount of caustic soda, has reduced the cost of product, and the process loss of raw material is few, helps improving the yield of product, and isolated stearate filter of resultant of reaction and water content are low, and filter cake is particle or coccoid.Carry out the exsiccant treatment process after adopting wet feed to pulverize and eliminated dust pollution and loss of material that drying and crushing produces, in stearic acid, finished product stearate yield is more than 98%.Dry easily, consume less calories, save the energy.Do not produce owing to there are other salts in the technology, inorganic salt content is low in the stearate product, helps improving the quality of products.
The inventive method also can be used for the preparation of the salt of other water-fast higher fatty acid such as acids such as Palmiticacid, naphthenic acid except that being used to prepare the stearate that metal oxide or oxyhydroxide is insoluble in water.
Be embodiments of the invention below, further specify the present invention by embodiment.
Embodiment 1:
Have in the enamel reaction still that the band of sealing cover stirs at 100 liters and to put into 80 liter water, start and stir 10 kilograms of back input stearic acid, be converted to 100% calcium oxide and be 1.05 kilograms calcium oxide or calcium hydroxide, tighten heated and stirred was reacted 50～70 minutes under 103～106 ℃ of conditions, venting after removing and pressing is filtered reactant, the gained filter is also pulverized the back by common drying means and condition drying, getting 10.5 kilograms of powder stearic acid calcium, is 98.1% with the stearic acid rate of collecting.
Embodiment 2:
Have in the enamel reaction still that the band of sealing cover stirs at 100 liters and to add 80 liter water, start and stir 10 kilograms of back input stearic acid, and be that 100% zinc oxide is 1.50 kilograms zinc oxide by content conversion, tighten and make behind the sealing cover under the situation that keeps airtight in the still stirring heating 106～108 ℃ of reactions 200～230 minutes, the reaction back venting that finishes removes and presses.Reactant filters the gained filter and pulverizes the back and carry out drying with usual method and condition, obtains 10.85 kilograms on powder stearic acid zinc, is 99% with the stearic acid rate of collecting.
Embodiment 3:
Have in the enamel reaction still that the band of sealing cover stirs at 100 liters and to add 80 liter water, start to stir and add 8 kilograms of stearic acid and by the hydrated barta of 4.65 kilograms of the barium hydroxides of content conversion 100%.Tighten and make behind the sealing cover under the situation that keeps airtight in the still stirring heating at 103～105 ℃.Reacted 60～80 minutes, reaction finishes the back venting except that pressing.Resultant of reaction filters, and obtains carrying out drying with common stearate drying means and condition after filter and the pulverizing, obtains 9.2 kilograms of powder stearic acid barium, and in stearic acid, yield is 99%.
Embodiment 4:
Have in the enamel reaction still that the band of sealing cover stirs at 100 liters and to add water 80 liters, starting 8 kilograms of stirring back input stearic acid and converting by content is that 100% plumbous oxide is 3.3 kilograms plumbous oxide, tighten the sealing cover post-heating and be stirred under 110～128 ℃ of conditions of temperature and reacted 210～230 minutes, the reaction back venting that finishes removes and presses.Resultant of reaction filters, and after obtaining filtering and pulverizing, carries out drying with usual method and condition, gets plumbous 12.2 kilograms of powder stearic acid, is 99% with the stearic acid rate of collecting.
Embodiment 5:
In having the enamel reaction still of stirring of sealing cover, 100 liters put into 80 liter water, start and stir that 8 kilograms of stearic acid are dropped in the back and by the Cadmium oxide of 1.9 kilograms of the Cadmium oxides of content conversion 100%, tighten the sealing cover post-heating and be stirred under 110～120 ℃ of conditions and reacted 210～230 minutes, the reaction back venting that finishes removes and presses.Resultant of reaction carries out centrifugation, and the gained filter is also pulverized the back and carried out drying with common stearate drying means and condition, obtains 8.9 kilograms of powder stearic acid cadmiums, is 99.% with the stearic acid rate of collecting.
Comparative example:
In 300 liter enamel reaction stills, add water 200 liters, start stirring heating and drop into 10 kilograms of stearic acid, the slow 20%(weight that adds when temperature rises to 85 ℃) sodium hydroxide is 7.5 kilograms, 95 ℃ are incubated saponification 30 minutes, be cooled to 90 ℃ then and slowly add the 15%(weight) 13.9 kilograms of calcium chloride waters, 85～95 ℃ of insulations were carried out replacement(metathesis)reaction 30 minutes, resultant of reaction moves into and removes mother liquor adding hot wash 2～3 times in the washing tank, carry out centrifugal dewatering after the washing, filter and drying, pulverize 10.3 kilograms of finished product calcium stearates, yield counts 96.3% with stearic acid.
Claims (6)
1, there is the manufacture method of the stearate that is insoluble in water in a kind of stearate molecule institute metal ion with oxide compound or oxyhydroxide form, it is characterized in that fineness is that the metal oxide of 200 mesh sieve all-pass or oxyhydroxide, stearic acid are put into feed intake weight and stearic acid of metal oxide or metal hydroxides and fed intake that 7～10 times of water of weight sum are airtight under the reactor stirring state to be warming up to 103～130 ℃ of reactions 60～230 minutes, the filter of resultant of reaction centrifugation gained and pulverize after carry out drying.
2, press the preparation method of the described stearate of claim 1, it is characterized in that said stearate is a calcium stearate, said metal oxide or oxyhydroxide are calcium oxide or calcium hydroxide, said water consumption is feed intake 8～10 times of gross weight of calcium oxide or calcium hydroxide and stearic acid, temperature of reaction is 103～108 ℃, and the reaction times is 60～70 minutes.
3, press the preparation method of the described stearate of claim 1, it is characterized in that said stearate is a Zinic stearas, said metal oxide or oxyhydroxide are zinc oxide, said water consumption is feed intake 7～9 times of gross weight of zinc oxide and stearic acid, temperature of reaction is 106～108 ℃, and the reaction times is 200～230 minutes.
4, press the preparation method of the described stearate of claim 1, it is characterized in that said stearate is a barium stearate, said metal oxide or oxyhydroxide are hydrated barta, the said water yield is feed intake 7～9 times of gross weight of stearic acid, hydrated barta, temperature of reaction is 103～106 ℃, and the reaction times is 60～80 minutes.
5, press the preparation method of the described stearate of claim 1, it is characterized in that said stearate is a lead stearate, metal oxide or oxyhydroxide are plumbous oxide, the reaction medium water yield is feed intake 8～10 times of gross weight of stearic acid, plumbous oxide, temperature of reaction is 110～128 ℃, and the reaction times is 210～230 minutes.
6, press the preparation method of the described stearate of claim 1, it is characterized in that said stearate is a cadmium stearate, metal oxide or oxyhydroxide are Cadmium oxide, the reaction medium water yield is feed intake 8～10 times of gross weight of stearic acid, Cadmium oxide, temperature of reaction is 110～120 ℃, and the reaction times is 200～230 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91109875 CN1071911A (en) | 1991-10-26 | 1991-10-26 | The preparation method of stearate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91109875 CN1071911A (en) | 1991-10-26 | 1991-10-26 | The preparation method of stearate |
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| CN1071911A true CN1071911A (en) | 1993-05-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 91109875 Pending CN1071911A (en) | 1991-10-26 | 1991-10-26 | The preparation method of stearate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1839111B (en) * | 2003-07-25 | 2010-04-21 | 普罗米蒂克生物科学公司 | Preparation of metal salts of medium-chain fatty acids |
| CN101486805B (en) * | 2008-11-20 | 2011-08-10 | 靖江旭光塑胶有限公司 | Preparation of calcium zinc composite stabilizer for processing plastic |
-
1991
- 1991-10-26 CN CN 91109875 patent/CN1071911A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1839111B (en) * | 2003-07-25 | 2010-04-21 | 普罗米蒂克生物科学公司 | Preparation of metal salts of medium-chain fatty acids |
| CN101486805B (en) * | 2008-11-20 | 2011-08-10 | 靖江旭光塑胶有限公司 | Preparation of calcium zinc composite stabilizer for processing plastic |
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