CN1050133C - Method for extracting and preparing biological preparation using chitin as raw material and application thereof - Google Patents
Method for extracting and preparing biological preparation using chitin as raw material and application thereof Download PDFInfo
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Abstract
The present invention discloses a method for extracting various chitin elements by using chitin as raw material. Various extracted chitin elements are proportionally prepared into various biological preparations. The biological preparations can be applied to the food field, the medicine field, the tobacco field, the paper making field, the textile field, the chemical industry field, etc. The present invention leads raw material to be soaked, degraded and separated in various kinds of inorganic solution, and finally, various products and side products are obtained. The present invention does not use organic solvent, pressurization is not required, and the raw material does not need to be pulverized. The present invention has the advantages of simple method, various obtained products, high purity of products, low preparation cost, no pollution, etc.
Description
The invention belongs to the chitin is the improvement that raw material extracts crust quality method, relates to the method that is prepared biotechnological formulation by it, and in the application of industries such as tobacco, food, medicine, chemical industry.
The alleged chitin of the present invention is for extracting the raw material of crust quality, be mainly Carapax Eriocheir sinensis, dried small shrimp, lobster skin of Crustachia class etc., the exoskeleton of the shell of also useful clam, inkfish, inner frame and tubercle animal is the report of raw material, and contained composition is referring to accompanying drawing 1 in the chitin; The crust quality is meant contained organism composition in the chitin; Chitin also claims chitin, is meant acetylize shell monose polymer; Chitosan also claims to restrain glycan, poly-gram sugar, chitosan, chitin quality, is meant deacetylation shell monose polymer; Rescue be apt to is the functional food that Japan develops more, is to be mixed by a certain percentage by chitin and chitosan; Dimension Kang Su is the specific address to the biotechnological formulation of the present invention's preparation, is the series product that mix by the different ratios preparation by the various organism that extract in the chitin.Since inconsistent in existing every profession and trade and the report to the address of above-mentioned substance, so define in this title to material involved in the present invention.
Saying of " doctor food homology " just arranged on the Ancient Times in China medical book, and in " Shiliao Bencao ", the Carapax Eriocheir sinensis tool is just the arranged argumentation of " main all heat of loosing, control stomach Qi, restoring and treating injured soft tissues arteries and veins, help digestion "; In " book on Chinese herbal medicine high former ", have " attack poison loose wind, long-pending, the row stasis of blood disappears " record of function.Chitin was single from coming out called after Funging from the mushroom class by French Bracomo in 1811; Odier also found this material, called after chitin in the insect incrustation in 1823; Spherical chitosan is to be found by French Rouget in 1859, is named in 1894.
In recent years, many developed countries have dropped into a large amount of funds and manpower to the development research of chitosan, and recognize that chitosan is human body indispensable " the 6th vital principle ", has caused people's common concern.Japan in 1993 the extraction industrialization of chitosan, and with its product application in industries such as medicine, chemical industry, environmental protection, food, its exploitation " rescue be apt to " puts on market as function of human body Sexual health promotion food.Up to now, people are to the study and cognition of chitosan, except that as also having following function the food.
Medical function has: the resistibility of reinforced immunological, raising body, and the generation and the development of anti-cancer, control cancer cell are used for the treatment of antianaphylaxis and various immunodeficiency diseasess; Regulate organism balance, treatment psychasthenia disease, Ginseng Extract; Anti-ageing, activation nutrition sarcostyle, prolongs life; Eliminate cylinder metabolism-ure, treat various metabolic diseases (as: uremia, diabetes, hyperlipidemia etc.); Can the interior external objectionable impurities (as agricultural chemicals, heavy metal, chemical pigment etc.) of adsorbent.A small amount of chitosan is blended in industrial application with chitin: be mainly used in aspects such as antiacid alkali, wear-resisting, high-low temperature resistant, raising smooth finish, increase snappiness, as plastics, rubber, paint, lubricating oil, weaving, leather etc.Chitin and chitosan are used alone or as a mixture aspect environmental protection to be had: water filtration purification, decontamination, prevent the function of radioactive rays.
And the research that people extract the crust quality has only the record of chitin and chitosan at present, and other contained compositions are only known existence, and the report of extraction is not arranged.Chinese patent 93111716.X discloses a kind of preparation method of chitin, and the chitin that is extracted belongs to intermediate product, does not obtain chitosan yet, and complex process, cost are higher.A kind of preparation method of chitosan has been introduced in the application of Chinese patent 96121759.6, its processing condition complexity, need pressurization, with an organic solvent, must pulverize raw material, thereby what obtain is single product.
In addition, the vitriol and the hydrochloride byproduct that form in chitosan extracts may have special performances, have become the easy-to-sell goods of America and Europe, south east asia at present, can be used for industries such as industrial or agricultural, medicine, food, cosmetic, printing and dyeing.
The purpose of this invention is to provide the easy chitosan extracting method of a kind of processing condition, enable to obtain contained material in the more raw materials, and the various extracts that will obtain are prepared into multiple biotechnological formulation and are applied.
Technical scheme of the present invention is as follows, earlier the chitin raw material is rinsed well, the NaOH solution of putting into 0.5-1% soaked 4-5 hour, pulling the hydrochloric acid soln of putting into 2-4% after the flushing again out soaked 18-24 hour, pulling the NaOH solution of putting into 30-50% after the flushing again out soaked 18-24 hour, pull the potassium permanganate solution of after flushing, putting into 2-8 ‰ again out and soaked 1-2 hour, put into the NaHSO of 1-3 ‰ after pulling out again
3After soaking 2-3 hour in the solution, pulling the NaOH solution of putting into 40-70% after the flushing again out soaked 18-24 hour under 45-70 ℃ of condition, obtain the chitin product after pulling flushing out, if pulling the NaOH solution of directly putting into 70-85% out soaked 5-7 hour under 140-170 ℃ of condition, pull flushing out and then obtain the chitosan product.
Feature of the present invention also is,, takes out its lower floor's solution and transfers PH to 5-6 with dilute sulphuric acid after repeatedly soaking use at the NaOH of above-mentioned 30-50% solution, then separates out the Saliva Orthana product; Surplus solution obtains multiple free amine group acid product by electrolysis; Again the surplus solution lyophilize is obtained the vitriol byproduct.The hydrochloric acid soln of above-mentioned 2-4% through repeatedly soak use after, take out the solution NaHCO of its lower floor
3Solution is transferred PH to 8-9, natural subsidence layering in a hour, and lower sediment is an inorganics, takes out at the middle and upper levels solution with middling speed centrifugal 10 minutes, and lower sediment is the organic active calcium product, and upper strata liquid is the mucopolysaccharide product, and middle level liquid is the hydrochloride byproduct.
Feature of the present invention also is, prepares multiple biotechnological formulation with the various crust quality that the present invention was extracted by the certain weight ratio mixing energy, and its corresponding use is arranged.
The chitosan of prescription 1:86-90% mixes with the organic active calcium of 10-14%, the powder that is white in color, tasteless, be dissolved in organic monoacid.The additive that can be used for food, beverage, healthcare products and toothpaste.
The citric acid of the chitosan of prescription 2:40-55%, the mucopolysaccharide of 15-25%, 30-40% mixes, and is light yellow viscous liquid, PH4-6.Be mainly used in the human body skin protective membrane and have carrier and matrix effect, replace used externally applied medicine matrix and cosmetic base; Can also be sprayed on Mouthpiece for cigarette substituted glycerol acid fat, improve the suction of smoke, reduction Nicotine, weaken the habituation of tobacco, strengthen the immunocompetence of breathing, Digestive tract.
The chitosan of prescription 3:20-25%, the mucopolysaccharide of 15-20%, the Saliva Orthana of 60-65% mixes, and is white powder, tasteless, refrigerant.Can be wrapped in the Mouthpiece for cigarette, adsorptive nicotine, to reduce the tar effect obvious, and mouthfeel is good; Can also add the smooth finish that improves paper in the paper pulp, have effect anticorrosion, mildew-resistant; Can also have the effect of removing halitosis, taking care of one's teeth, suppressing the germ growth as the additive of toothpaste.
The organic active calcium of prescription 4:15-20% chitosan, 60-65%, the Saliva Orthana of 16-20% mix, and powder is white in color.Be wrapped in the Mouthpiece for cigarette, have the effect of adsorptive nicotine, reduction tar, clean taste is to pharyngeal non-stimulated.
The amino acid of the chitosan of prescription 5:80-85%, the organic active calcium of 10-16%, 4-10% mixes, and powder is white in color.The effect that is used for medicine and has Ginseng Extract, helps growth, improves immunizing power; The additive that also can be used for functional food.
The chitosan of prescription 6:40-45%, the amino acid of 30-35%, 20-30% organic active calcium mix, and powder is white in color.Be used for medicine and have the promotion union of fracture, anti-curing hyperosteogeny, osteoporotic function.
The chitin of prescription 7:80-97% mixes with the Saliva Orthana of 3-20%, and powder is white in color.Be used for the pulling force that textiles can improve fiber; In lubricating oil, paint, rubber, can prevent to wear out, anticracking, the antiacid alkali of tool, attrition resistant effect; And can in the making of disposable tableware, plastic film, add on a small quantity, make it easy to decompose, be beneficial to environmental protection.
From such scheme as can be seen, crust quality extracting method of the present invention, not with an organic solvent, need not pressurize, raw material need not be pulverized, simple, and can obtain multiple crust quality product and byproduct, thereby production cost is reduced greatly, and the purity of chitosan can reach 99.2%, and yield reaches 12%, whole leaching process non-environmental-pollution problem; The multiple biotechnological formulation that the various crust quality of being extracted are made in proportion, can use in fields such as food, medicine, tobacco, papermaking, weaving, chemical industry.
Accompanying drawing 1 is a contained composition synoptic diagram in the chitin; Accompanying drawing 2 is the schematic flow sheet that raw material extracts various crust quality products and byproduct with the chitin for the present invention, and frame of broken lines is the finished product among the figure; Accompanying drawing 3 for the prepared several biotechnological formulations of the present invention after using on the Mouthpiece for cigarette, the curve synoptic diagram of coal-tar middle oil content of its cigarette smoke and biotechnological formulation add-on.Dimension Kang Su II, corresponding the doing among the present invention of III, IV fill a prescription 2,3,4 in the accompanying drawing 3; As can be seen from the figure, the dimension Kang Su that adds 1 milligram in every cigarette just makes tar content obviously reduce, reduce the tar ability convergence limit when reaching 4 milligram hours, so the dimension Kang Su add-on of every cigarette is at the 2-4 nanogram range, dimension Kang Su adding method on Mouthpiece for cigarette is, liquid preparation can be sprayed directly on on the mouth rod, or alternative R-Glyceric acid fat adds when system mouth rod; Powder formulation then can evenly be wrapped in the mouth rod, or the absorption interlayer that places the mouth rod to be provided with.Learn after testing that in addition Kang Su is added on the Mouthpiece for cigarette dimension, can also reduce the content of nicotine and total particulate matter in the flue gas.
Below describe some problems in the concrete enforcement of technical solution of the present invention in detail.
Get 1 kilogram of chitin raw material of rinsing well (then be called for short shell material), being immersed in the NaOH solution of 0.5-1% has bubble to produce, and is toxin and the impurity of sloughing shell material surface, takes out water when no bubble produced at 4-5 hour and washes; Dropping into has bubble to produce again in the HCl solution of 2-4%, normal temperature soaks 18-24 hour no bubble down and produces the back taking-up, show that acetate fat, organic calcium, mucopolysaccharide, inorganics etc. are dissolved in the acid solution fully, put into NaOH solution 18-24 hour of 30-50% after the flushing again, degrade proteins, dissolving Saliva Orthana, take out when the attenuation of shell material is translucent, this moment, the composition of shell material was the acetylize chitin; After flushing, insert in the potassium permanganate solution of 2-8 ‰ and soaked 1-2 hour, take out when making the shell material be brownish black, put into the NaHSO of 1-3 ‰ again
3Soaked 2-3 hour in the solution, make polysaccharide be converted into monose, the shell material bleaches fully, and take out the back and flushing; Insert again in the NaOH solution of 40-70% and under 45-70 ℃ of condition, soaked 18-24 hour, the sensation that the shell material tears paper-tear picture with hand, promptly polyreaction finishes, and after taking out the shell material and rinsing drying well and pulverize, becomes the chitin product; If with putting into the NaOH solution of 70-85% after the taking-up of shell material again, soaked 5-7 hour under 140-170 ℃ of condition, taking-up becomes the chitosan product after rinsing the drying pulverizing well.The survey method of analysing of chitosan purity is, uses 10% citric acid (or using Glacial acetic acid, lactic acid etc.) solution soaking, and chitosan can dissolve in 30 minutes fully, and nonsoluble is a chitin.The chitosan purity of extracting by above-mentioned requirements is 99.2%, and yield is 12%.
In above-mentioned steps, the concentration and the soak time of employed various soak solutions are inversely proportional to, and be not strict to the concentration requirement of each solution in other words, and concentration is low, and then soak time is long, and concentration height then soak time is short; Requirement to temperature also is like this; And the selection to each solution reagent is not strict with yet, and some reagent can adopt other reagent to replace, as replacing NaHSO with oxalic acid
3And these all should belong in protection scope of the present invention.
In aforementioned mucinous extraction, after Saliva Orthana is separated out, take out drying and dehydrating and be the Saliva Orthana product; Its yield can reach 2%; Surplus solution transfers to amino acid whose iso-electric point, obtains multiple total free aminoacids by electrolysis, is product after the drying dehydration, and its yield can reach 2%; Crystal vitriol byproduct will be obtained again behind the surplus solution drying and dehydrating.In the extraction of aforementioned mucopolysaccharide, middling speed is centrifugal to be 1600-2000 rev/min, and three kinds of products that obtain after centrifugal all need drying and dehydrating, and wherein the mucopolysaccharide yield can reach 3%, and organic active calcium yield is 40%.
The various biotechnological formulations that the present invention is prepared, the contriver is called dimension Kang Su, its dimension Kang Su I, II, III, corresponding to above-mentioned prescription 1,2,3.The contriver tries out prepared dimension Kang Su series product in some industries, received obvious effects.
Claims (1)
1. method for preparing chitosan, be to be raw material with Carapax Eriocheir sinensis, dried small shrimp or lobster skin, it is characterized in that, earlier raw material is rinsed well, put in the NaOH solution of 0.5-1% (weight) and soaked 4-5 hour, pulling the hydrochloric acid soln of putting into 2-4% (weight) after the flushing again out soaked 18-24 hour, pulling the NaOH solution of putting into 30-50% (weight) after the flushing again out soaked 18-24 hour, pull the potassium permanganate solution of after flushing, putting into 2-8 ‰ (weight) again out and soaked 1-2 hour, put into the NaHSO of 1-3 ‰ (weight) after pulling out again
3Soaked 2-3 hour in the solution, pulling the NaOH solution of putting into 40-70% (weight) after the flushing again out soaked 18-24 hour under 45-70 ℃ of condition, pull the flushing back out and be chitin, put it in the NaOH solution of 70-85% (weight), under 140-170 ℃ of condition, soaked 5-7 hour, pull flushing again out and then obtain the chitosan product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97108700A CN1050133C (en) | 1997-06-20 | 1997-06-20 | Method for extracting and preparing biological preparation using chitin as raw material and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN97108700A CN1050133C (en) | 1997-06-20 | 1997-06-20 | Method for extracting and preparing biological preparation using chitin as raw material and application thereof |
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| CN1167117A CN1167117A (en) | 1997-12-10 |
| CN1050133C true CN1050133C (en) | 2000-03-08 |
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| CN97108700A Expired - Fee Related CN1050133C (en) | 1997-06-20 | 1997-06-20 | Method for extracting and preparing biological preparation using chitin as raw material and application thereof |
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| CN108395588A (en) * | 2018-01-17 | 2018-08-14 | 宁国市顺鑫金属制品有限公司 | The strong forging press cushion pad and preparation method thereof of wear-resistant antibacterial ability |
| CN111378210A (en) * | 2020-03-24 | 2020-07-07 | 安徽中烟工业有限责任公司 | Preparation method of ternary metal MOFs-chitosan composite material and application of ternary metal MOFs-chitosan composite material in reducing harm of cigarette smoke |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH05279401A (en) * | 1992-03-31 | 1993-10-26 | Nippon Kayaku Co Ltd | Production of powdery chitosan |
| CN1085564A (en) * | 1993-08-20 | 1994-04-20 | 连云港开发区金祥贸易有限公司 | A kind of preparation method of chitin |
| CN1089620A (en) * | 1993-12-15 | 1994-07-20 | 屈步华 | Preparation method and product with natural structure chitin |
| CN1126048A (en) * | 1995-05-06 | 1996-07-10 | 陈松伟 | Textured vegetable protein containing chitin and its derivatives and prepn. method thereof |
| CN1138336A (en) * | 1994-12-02 | 1996-12-18 | 汉克尔股份两合公司 | Cationic biopolymers |
-
1997
- 1997-06-20 CN CN97108700A patent/CN1050133C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH05279401A (en) * | 1992-03-31 | 1993-10-26 | Nippon Kayaku Co Ltd | Production of powdery chitosan |
| CN1085564A (en) * | 1993-08-20 | 1994-04-20 | 连云港开发区金祥贸易有限公司 | A kind of preparation method of chitin |
| CN1089620A (en) * | 1993-12-15 | 1994-07-20 | 屈步华 | Preparation method and product with natural structure chitin |
| CN1138336A (en) * | 1994-12-02 | 1996-12-18 | 汉克尔股份两合公司 | Cationic biopolymers |
| CN1126048A (en) * | 1995-05-06 | 1996-07-10 | 陈松伟 | Textured vegetable protein containing chitin and its derivatives and prepn. method thereof |
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| CN1167117A (en) | 1997-12-10 |
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