CN1058259C - Method for preparation low-salt compound amino-acid powder by cystine mother solution and its equipment - Google Patents
Method for preparation low-salt compound amino-acid powder by cystine mother solution and its equipment Download PDFInfo
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- CN1058259C CN1058259C CN96117556A CN96117556A CN1058259C CN 1058259 C CN1058259 C CN 1058259C CN 96117556 A CN96117556 A CN 96117556A CN 96117556 A CN96117556 A CN 96117556A CN 1058259 C CN1058259 C CN 1058259C
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Abstract
The present invention discloses a method and equipment for preparing low-salt compound amino-acid powder from a cystine mother solution, which is characterized in that the method comprises: placing the cystine mother solution in a crystallisation tank provided with an adsorption medium frame, depositing and crystallizing for 3 to 10 hours at subzero 5 to subzero 20 DEG C, depressurizing and concentrating the filtered solution to 20 to 25 Be, and drying by spraying. The method can enable the recovery rate of amino acid to be higher than 90%, the content of chlorinated ammonium chloride in the product is only 25%, and the content of amino acid is higher than 65%. After pilot scale production, the present invention not only favorably solves the problem of environmental pollution by the cystine mother solution, but also enlarges protein sources of the stall food for animals; the present invention has favorable social benefit and high economic benefit.
Description
The invention belongs to the amino acid production technical field, especially a kind of method of preparation low-salt compound amino-acid powder by cystine mother solution and equipment thereof.
At present, Gelucystine production all is to utilize Keratin sulfate in the animal hair, through the concentrated hydrochloric acid heating hydrolysis, the minimum principle of solubleness when utilizing the material iso-electric point, ammonification is neutralized to the iso-electric point of Gelucystine in hydrolyzed solution, makes it emanate from hydrolyzed solution, through purifying technique, obtain the Gelucystine crystal again.Hydrolyzed solution behind the extraction Gelucystine is a mother liquor, and it contains multiple amino acids and a large amount of ammonium chlorides, because ammonium salt is difficult to separate from mother liquor, thereby, most of producers make waste directly to the rivers discharging with mother liquor, have both wasted valuable animal protein resource, have polluted environment again.Form in order to reduce the ammonium chloride that is difficult in the Gelucystine production process rejecting, partly producer once adopted thickening equipment to catch up with acid, to reduce the excessive hydrogen chloride in the hydrolyzed solution, reduced excessive hydrochloric acid and neutral ammonia and generated ammonium salt.But because hydrochloric acid was its aqueous solution constant boiling point at 20.22% o'clock, can't reach the purpose of independent disacidify, also this equipment complexity, and acid corrosion is serious, fails to be promoted application.The more domestic Biochemie Gesellschaft m.b.H. (AU) A-6250 Kundl, Austria of the seventies have carried out big quantity research to the utilization of mother liquor, as the auxiliary reagent factory, Wuhan take the lead in mother liquor by spraying drying produce " compound amino-acid powder " but since in the finished product ammonium chloride content surpass 50%, each seed amino acid total content only is about 38%, its use range is subjected to great restriction, thereby product is not by social recognition.Domestic in recent years part producer adopts first concentrated mother liquor, and partly ammonium chloride is rejected in crystallization under normal temperature condition, with the capable spraying drying of surplus liquid, makes " compound amino-acid powder " again.Its concrete technology is that mother liquor is at first through concentrating under reduced pressure, make strength of solution bring up to 22～25Be, concentrated solution is placed in the open type crystallizer tank, (about 15 ℃) crystallization under the normal temperature condition by 10～17Be (Bo Meishi degree), separate out partly ammonium chloride, again with the capable spraying drying of surplus liquid.Above-mentioned technology, in the mother liquor concentration process, variation has taken place in various solute concentrations simultaneously, and ammonium chloride has improved concentration relatively, has reached supersaturation in mother liquor, ammonium chloride particle unsteady state occurs, through the particle movement collision, draws close, and nucleus occurs; After mother liquor concentrates, reduced water as solvent, certain variation has also taken place in mother liquor PH, each seed amino acid also changes along with concentration ground and the change of pH value, motion and collision also appear in the particle of 16 seed amino acids to some extent, but have little time to arrange well, can only be subjected to continuing influence by the unstable particle of border facial mask by rule, form new nucleus or be attached to brokenly generate on the nucleus pseudo-brilliant; Contain colloidal impurity in the mother liquor,, the boundary film is thickened owing to concentrate the concentration that has increased colloidal impurity relatively, hinder the diffusion of ammonium chloride particle, the ammonia chloride crystal coarsening rate is descended, a plurality of nucleus occur, form Powdered crystallisate, reduced the eduction rate of ammonium chloride.Meanwhile colloidal impurity is because change in electrical charge also along with the pseudo-crystalline substance of each seed amino acid, ammonium chloride powder crystal are separated out jointly, causes amino acid rate of recovery decline in the mother liquor, and ammonium chloride content is still more than 39% in the gained aminoacids complex.
The objective of the invention is to overcome the deficiencies in the prior art, compounded amino acid recovering rate in a kind of raising cystine mother liquor is provided, reduce the production method and the equipment thereof of the low-salt composite aminophenol of ammonium chloride content in the aminoacids complex, use method of the present invention, the compounded amino acid recovering rate can reach 90% in the Guang amino acid mother liquor, and ammonium chloride content can be reduced to about 25% in the compound amino-acid powder product.
Purpose of the present invention realizes by following technical proposals:
Cystine mother liquor places the crystallization case, insert absorption amboceptor support again, under-5～-20 ℃ of conditions, left standstill crystallization 3～10 hours, filter solid-liquid two is separated, collect filtrate and carry out concentrating under reduced pressure to 20～25Be, insert again and carry out spraying drying, packing in the spray-drying tower.
The crystallization case is the rectangular box that heat conductivility preferred metal sheet material is made, bottom half is equipped with roller or pole, roller is connected with casing by support, and box inside is provided with anticorrosion lining, and said anticorrosion lining is Resins, epoxy, furane resin coating layer or is pasted with the plastics lamella.Casing top is provided with suspension rod, the draw-in groove clamping affixed or that be provided with casing of suspension rod and casing top row.
The present invention mainly is two physical propertiess having utilized ammonium chloride; At first be to utilize the solubleness of ammonium chloride to be directly proportional with temperature, its solubleness and temperature relation such as table 1:
The relation of table 1 chloride leach degree and temperature
| Temperature (℃) | -20 | -10 | 0 | 10 | 20 | 30 | 40 |
| Solubleness (%) | 20 | 25 | 29.4 | 33.3 | 37.2 | 41.4 | 45.8 |
Be under the cryogenic situation at mother liquor, the solubleness straight line of ammonium chloride descends, ammonium chloride is hypersaturated state in the mother liquor, gravitation between the ammonium chloride particle is greater than the magnetism of solution to it, the ammonium chloride particle is in unsettled upper state, they are drawn close each other, run foul of each other in the motion, nucleus occurs, through moving repeatedly, colliding, attract, draw close, disperse, arrange, assemble, emit heat energy, and arrange according to certain rules, polymerization and crystallization is separated out, this not only greatly reduces the content of ammonium chloride in the mother liquor, and has reduced various amino acid whose losses.Because amino acid and ammonium chloride molecular structure, physicochemical property differ greatly, and the concentration and the pH value of mother liquor do not change, thus at ammonium chloride in whole crystallisation process, each seed amino acid is used as impurity and discharges outside the ammonia chloride crystal.Next is characteristics of utilizing ammonium chloride to have moisture absorption to lump slightly, makes crystal become block.Under cold condition, behind the ammonium chloride crystals, crystal crystallizes into caking very soon.Utilize various absorption amboceptors to make the thing that depends on of nucleus, but the accelerate crystallisation process, its caking characteristics in addition, thus reach the purpose that ammonia chloride crystal becomes piece to separate out.
From above-mentioned situation as can be known, the objective of the invention is to realize, through lab scale and middle trial production, effect is all good.Low temperature process gained ammonium chloride product and aminoacids complex quality product all are better than the normal temperature method, see table 2, table 3 for details.
Table 2 normal temperature method and low temperature process gained compound amino-acid powder mass ratio are
| Method | The normal temperature method | Low temperature process |
| Total amino acid content (%) | 50～52 | ≥65％ |
| NH 4CL content (%) | 39±2 | 25±2 |
| Moisture content (%) | 2±0.5 | 2±0.5 |
| Ammonia, arsenic, lead | Up to standard | Up to standard |
Table 3 normal temperature method and low temperature process gained ammonium chloride mass ratio are
| Method | The normal temperature method | Low temperature process |
| Product appearance | Grey black crystalline flour end and colloidal mixture | The yellow crystals ingot |
| NH 4CL content (%) | 63±2 | ＞90 |
| Moisture content (%) | 18±2 | ＜5 |
Accompanying drawing 1 is faced configuration diagram for crystallization case of the present invention;
Accompanying drawing 2 is crystallization case side-looking configuration diagram of the present invention;
In conjunction with the embodiments the present invention is further described with reference to the accompanying drawings below:
Example I is got cystine mother liquor and is placed the crystallization case, as Fig. 1, shown in Figure 2, the crystallization case is the rectangular box that heat conductivility preferred metal sheet material is made, the casing size designs as required, generally should consider to enlarge mother liquor and cold environment contact surface as far as possible and come in and go out refrigeration chamber conveniently, present embodiment casing length * wide * height is 100cm * 30cm * 30cm.Bottom half dress roller 1 or pole, roller is connected with casing 3 by support 2, and is unsettled to guarantee crystallization case bottom, lowers the temperature as early as possible in order to mother liquor.Cabinet wall is provided with the anticorrosion lining 4 of one deck, moulds lamella as Resins, epoxy, furane resin or stickup skim, and anticorrosion lining surface should be smooth smooth, crystallizes into piece with the attached wall of preventing ammonium chloride, is difficult to take out, and present embodiment selects for use the furans coating to serve as a contrast.Casing top is provided with suspension rod 5 and box body wall top clamping or affixed, and present embodiment is selected for use affixed, and suspension rod is provided with ties up hook 6, so that be connected with the absorption amboceptor.To adsorb amboceptor again and be bundled in tying up on the hook of crystallization casing top, said absorption amboceptor is the vegetable fibre rope, net or shaggy steelframe are good, the absorption amboceptor should be suspended from the mother liquor, preventing to adsorb amboceptor contacts more with case under casing wall, in order to avoid the ammonium chloride crystal block is difficult for taking out, present embodiment is selected the rope made of hemp for use, again the crystallization case is placed refrigerator compartment, leave standstill crystallization, freezer temperature is good with-5～-20 ℃, and present embodiment is selected-5 ℃ for use, time of repose was good with 3～10 hours, present embodiment was selected for use 3 hours, took out the crystallization case, filtered solid-liquid separation by 10 order filter clothes, collect filtrate and be evaporated to 20～28Be, present embodiment is selected for use and is concentrated into 25Be, inserts and carries out spraying drying, packing in the spray-drying tower.
Example II is got cystine mother liquor and is placed the crystallization case, the crystallization case is the rectangular box that heat conductivility preferred metal sheet material is made, the casing size designs as required, generally should consider to enlarge mother liquor and cold environment contact surface as far as possible and come in and go out refrigeration chamber conveniently, present embodiment casing length * wide * height is 100cm * 40cm * 30cm.Four on bottom half dress roller, roller is connected with casing by support, and is unsettled to guarantee crystallization case bottom, lowers the temperature as early as possible in order to mother liquor.Cabinet wall is provided with the anticorrosion lining of one deck, and present embodiment is selected PVC plastic plate lining for use.Again the adsorptive amboceptor is placed the tying up on the hook of suspension rod on the binding crystallization casing, said absorption amboceptor is the smart rough steelframe in surface, the absorption amboceptor should be suspended from the mother liquor, preventing to adsorb amboceptor contacts more with case under casing wall, in order to avoid the ammonium chloride crystal block is difficult for taking out, again the crystallization case is placed refrigerator compartment, leave standstill crystallization, freezer temperature is good with-5～-20 ℃, present embodiment is selected-10～-12 ℃ for use, when leaving standstill with 3～10 hours for good, present embodiment was selected for use 6 hours, take out the crystallization case, filter solid-liquid separation by 10 order filter clothes, collect filtrate and be evaporated to 20～28Be, present embodiment is selected for use and is concentrated into 28Be, insert again and carry out spraying drying, packing in the spray-drying tower.
EXAMPLE III is got cystine mother liquor and is placed the crystallization case, the crystallization case is the rectangular box that heat conductivility preferred metal sheet material is made, the casing size designs as required, generally should consider to enlarge mother liquor and cold environment contact surface as far as possible and come in and go out refrigeration chamber conveniently, present embodiment casing length * wide * height is 100cm * 30cm * 40cm.Bottom half is equipped with pole, and is unsettled to guarantee crystallization case bottom, lowers the temperature as early as possible in order to mother liquor.Cabinet wall is provided with the anticorrosion lining of one deck, and present embodiment is selected Resins, epoxy coating lining for use.Again the adsorptive amboceptor is placed the tying up on the hook of binding crystallization casing top, or will adsorb amboceptor earlier and be bundled in and tie up on the hook, place cystine mother liquor again, said absorption amboceptor is a vegetable fibre netting, the absorption amboceptor should be suspended from the mother liquor, preventing to adsorb amboceptor contacts more with case under casing wall, in order to avoid the ammonium chloride crystal block is difficult for taking out, again the crystallization case is placed refrigerator compartment, leave standstill crystallization, freezer temperature is good with-5～-20 ℃, present embodiment is selected-18～-20 ℃ for use, and time of repose was good with 3～10 hours, and present embodiment was selected for use 10 hours, take out the crystallization case, filter solid-liquid separation by 10 order filter clothes, collection filtrate is reduced pressure and is contracted deeply to 20～28Be, and present embodiment is selected for use and is concentrated into 20Be, insert again and carry out spraying drying, packing in the spray-drying tower.
Claims (3)
1, a kind of method of preparation low-salt compound amino-acid powder by cystine mother solution comprises that ammonia salts out and the drying process with atomizing process, is characterized in that: undertaken by follow procedure and method; Cystine mother liquor is placed the crystallization case, the crystallization case places under-5～-20 ℃ of conditions and left standstill crystallization 3～10 hours, carries out solid-liquid two by filtration and is separated, and collects filtrate, and filtrate decompression is concentrated into 20～28Be, insert again and carry out spraying drying, packing in the spray-drying tower.
2, according to the method for the said preparation low-salt compound amino-acid powder by cystine mother solution of claim 1, it is characterized in that: earlier natural fiber rope, net are hung in the crystallization case, again cystine mother liquor is placed the crystallization case, or earlier cystine mother liquor is placed the crystallization case, again natural fiber rope, net are hung in the crystallization case, the crystallization case places under-5～-20 ℃ of conditions and left standstill 3～10 hours, carrying out solid-liquid two by filtration is separated, collect filtrate, and filtrate decompression is concentrated into 20～28Be, place spray-drying tower to carry out spraying drying, packing again.
3, a kind of cystine mother liquor is produced the specific equipment of low-salt composite aminophenol, comprise with natural fiber rope, net and crystallization case, the crystallization case is the rectangular box that the sheet metal of good heat conductivity is made, the bottom half outside is provided with and guarantees unsettled roller or the pole in crystallization case bottom, roller is connected with casing by support, cabinet wall is provided with the anticorrosion pad of one deck, and anticorrosion lining is Resins, epoxy coating layer or furane resin coating layer or pastes one deck thin plastic sheet layer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117556A CN1058259C (en) | 1996-05-13 | 1996-05-13 | Method for preparation low-salt compound amino-acid powder by cystine mother solution and its equipment |
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|---|---|---|---|
| CN96117556A CN1058259C (en) | 1996-05-13 | 1996-05-13 | Method for preparation low-salt compound amino-acid powder by cystine mother solution and its equipment |
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| CN1144799A CN1144799A (en) | 1997-03-12 |
| CN1058259C true CN1058259C (en) | 2000-11-08 |
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| CN96117556A Expired - Fee Related CN1058259C (en) | 1996-05-13 | 1996-05-13 | Method for preparation low-salt compound amino-acid powder by cystine mother solution and its equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343194B (en) * | 2008-09-04 | 2011-06-15 | 湖北新生源生物工程股份有限公司 | Process for preparing low-salt composite aminophenol powder |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI123279B (en) * | 2011-06-17 | 2013-01-31 | Esko Viholainen | Virike Equipment |
| CN114455607B (en) * | 2022-03-08 | 2023-04-25 | 重庆工贸职业技术学院 | Purification method of industrial byproduct ammonium chloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1016768B (en) * | 1987-04-01 | 1992-05-27 | 海德堡印刷机械股份公司 | Paper sucking machine with lifting head |
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1996
- 1996-05-13 CN CN96117556A patent/CN1058259C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1016768B (en) * | 1987-04-01 | 1992-05-27 | 海德堡印刷机械股份公司 | Paper sucking machine with lifting head |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343194B (en) * | 2008-09-04 | 2011-06-15 | 湖北新生源生物工程股份有限公司 | Process for preparing low-salt composite aminophenol powder |
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| CN1144799A (en) | 1997-03-12 |
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