CN101407555A - Novel industrialized production technique of carboxymethyl pachyman - Google Patents
Novel industrialized production technique of carboxymethyl pachyman Download PDFInfo
- Publication number
- CN101407555A CN101407555A CNA2007100535482A CN200710053548A CN101407555A CN 101407555 A CN101407555 A CN 101407555A CN A2007100535482 A CNA2007100535482 A CN A2007100535482A CN 200710053548 A CN200710053548 A CN 200710053548A CN 101407555 A CN101407555 A CN 101407555A
- Authority
- CN
- China
- Prior art keywords
- solution
- sodium hydroxide
- tuckahoe
- carboxymethylpachymaran
- 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.)
- Pending
Links
Images
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a continuous industrialization production novel technique of ethyloic tuckahoe polysaccharide, and the main process is that edible alcohol is used for extracting pachymic acid and triterpenoid matters in tuckahoe powders to be as a tuckahoe extracting material and a tuckahoe alcohol material, and sodium hydroxide solution is used for alkalifying the tuckahoe powders extracted by the alcohol, a solution (1) is obtained by filtering and removing alkali insoluble matters in the tuckahoe, a solution (2) is obtained by neutralizing a chloroacetic acid solution by the sodium hydroxide solution, (1) is added in (2) while stirring, and the sodium hydroxide solution is added to lead the ethyloic reaction to carry out completely. The filtered solution is alkaline, is bleached by adding oxydol and is neutralized to neutrality by adding acetic acid or hydrochloric acid. The ethyloic polysaccharide finished product can be obtained by electrodialysing and removing impurities in the neutralized solution and spray drying the purified CMP solution. The invention combines the product producing and the product refining felicitously to obtain products by spray drying, and the CMP industrialization production is realized.
Description
Technical field
The invention belongs to natural macromolecule amylose class field, relate to and a kind of pachyman (Pachyman) is degraded into Pachymose (Pachymaran), carry out chemically modified etherification reaction synthesizing water-solubility carboxymethylpachymaran (Carboxy methyl pachymaran, production technique CMP) again.
Background technology
The research report, carboxymethylpachymaran (CMP) has the obvious suppression effect to mouse tumor U～14, S～180 sarcomas and liver cancer H22, can strengthen immune function of mice, can also induce people's blood lymphocyte to produce natural cell active factors such as Interferon, rabbit, interleukin-, tumour necrosis factor and granulocyte-macrophage colony-stimulating factor.Has application prospect as the anti-tumor biological reaction control agent.
People such as Hamuro synthesized CMP in 1971 first in the laboratory, this explained hereafter CMp needs a large amount of reagent such as ether, methyl alcohol, acetone, acetic acid and ethanol, is difficult to realize suitability for industrialized production, and environment is caused certain pollution.
The patent CN1554667A report of people such as Chen Chunxia application in 2003, employing water is medium, the static carboxymethylation of carrying out Pachymose of liquid phase.With products production with refining be divided into two operations and carry out, analyse by twice alcohol of twice neutralization of product by traditional method for this technology, and the production time is long, raw material acid, alkali consumption are big, particularly to analyse the consumption amount of alcohol very big for twice alcohol, and power consumption is big, still is difficult to realize large-scale industrial production.
Summary of the invention
The purpose of this invention is to provide a kind of carboxymethylpachymaran novel industrialized production technique, to adapt to large-scale industrial production.
Technical scheme of the present invention is: with synthetic and refining ingenious the combining of CMP, by the electrodialytic method purified product, obtain finished product with spraying drying.
The chemical reaction of synthetic carboxymethylpachymaran be a mol-chloric acetate with Pachymose in hydroxyl (OH) combine generation carboxymethylpachymaran sodium salt, consume two molecule NaOH:
〔C
6H
7O
2(OH)
3〕
n+2nNaOH+nClCH
2COOH→
〔C
6H
7O
2(OH)
2(OCH
2COONa)〕
n+nNaCl+nH
2O
In etherification reaction, NaOH and ClCH
2The COOH reaction generates an intermediate earlier, and this intermediate can generate CMP with the reaction of Pachymose sodium salt, also can generate the by product hydroxyethanoic acid with the NaOH effect:
When NaOH amount in the system surpasses when a certain amount of, the easier generation of this side reaction, therefore, NaOH and ClCH
2The COOH mole ratio is 2～2.13: 1 o'clock, and CMP output is the highest, and (D, S) is also bigger for substitution value.
80 order Poria powder are dissolved into pachymic acid and triterpene substance in the alcohol through the edible ethanol lixiviate, can be used as Poria cocos medicinal extract raw material or tuckahoe wine raw material.Foam when reducing the Pachymose alkalization reduces system's viscosity, is convenient to operation.
Pachymose is after carboxymethylation, and solution system is alkalescence (pH=11～12), just in time meets the hydrogen peroxide decolorization condition, and normal temperature decoloured more than 10 hours, and the back is used in the hydrochloric acid and pH=6.5～7.5.
After the decolouring neutralization, directly enter electrodialysis system.The sodium-chlor that in the Pachymose carboxymethylation reaction, produces, sodium chloroacetate and hydroxyethanoic acid sodium and with in the hydrochloric acid and the time sodium-chlor that produces, these salt can be removed by electrodialysis, make sodium-chlor in the finished product (NaCl) (%)＜0.01.
Get to spray-dryer high speed centrifugation dish by electrodialysis solution, by droplet and the reverse contact heat-exchanging of hot blast that centrifugal pan throws away, temperature is controlled at 103～105 ℃, gets white powder, and packing is dispatched from the factory.
Carboxymethylpachymaran industrialized producing technology provided by the present invention, by optimization of process conditions, the Controlling System water consumption, the electrodialytic method desalting purifying is used in the basic solution decolouring behind the carboxymethyl, and spraying drying simplifies the operation process greatly, without the alcohol precipitating.CMP per ton saves 10 tons of alcohol, and energy consumption reduces by 60%, reduces production costs greatly, realizes suitability for industrialized production.
The invention will be further described below in conjunction with accompanying drawing.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Poria cocos 50Kg pulverizes, and crosses 80 mesh sieves, puts in the 500L lixiviate still, adds 95% alcohol 150Kg, lixiviate 16 hours, and centrifuging, filtrate is made Poria cocos medicinal extract or tuckahoe wine raw material, and filter cake is continued to employ.
At 1000L1
#In the reactor, add the 600L pure water, 20KgNaOH is dissolved in wherein.Under stirring state, the Poria cocos filter cake smashed to pieces is added wherein dissolving alkalization 1～2 hour, through high speed centrifugation, the alkali insolubles of elimination about 4%, separate solution 1..
At 3000L2
#In the reactor, add the 500L pure water, wherein with the dissolving of 94.5Kg Mono Chloro Acetic Acid.Under stirring state, add (4mol/L) NaOH solution 200L and get solution 2., add NaOH solution (4mol/L) 150L again, the logical vapor temperature of chuck rises to 75～85 ℃, is incubated 4 hours.Normal temperature centrifuging, waste, filtrate is squeezed in the decolouring still, adds hydrogen peroxide 1600ml, and normal temperature decolours more than 10 hours.The back with hydrochloric acid add and, pH is transferred to 6.5～7.5.
Normal temperature is squeezed into the JX-D-VI electrodialysis system with neutralizer with pump, by anion and cation exchange membrane, removes 90% salinity, and product NaCl content is reached below 0.1%.Demineralised liquid is squeezed into spray-dryer high speed centrifugation dish with high-pressure pump, and feed liquid throws away and reverse hot blast contact heat-exchanging with the droplet state, and 103～105 ℃ of temperature controls reach below 8% CMP moisture.Gained white powder packing is dispatched from the factory.
The carboxymethylpachymaran white powder, odorless, tasteless.
pH＝5.0～7.0；
Moisture content (%)＜8;
Sodium-chlor (%)＜0.1%;
The total arsenic of heavy metal (in As) (%)＜0.001;
Total lead (in Pb) (%)＜0.005.
Claims (3)
1, a kind of novel industrialized production technique of carboxymethylpachymaran, it is characterized in that it being earlier with pachymic acid and triterpene substance in 2.5 times of edible ethanol extraction Poria powder, as Poria cocos medicinal extract raw material, the tuckahoe wine raw material, then with the Poria powder of sodium hydroxide solution alkalization through alcoholic extract, 1. the alkali insolubles that removes by filter in the Poria cocos gets solution, chloroacetic acid solution through sodium hydroxide solution neutralize solution 2., in under condition of stirring, will 1. adding 2., and add stoichiometric sodium hydroxide solution, the control reaction conditions, stir synthetic carboxymethylpachymaran, its main technique condition is:
The ratio of sodium hydroxide and Poria cocos dry powder is 1.68～1.70: 1.0
Wherein: sodium hydroxide and Mono Chloro Acetic Acid mole ratio are 2～2.13: 1.0
Dried Poria powder and water weight ratio are 1: 3～4
Alkalization time: 1～2 hour
75～85 ℃ of carboxymethylation temperature, 4 hours time.
2, the novel industrialized production technique of carboxymethylpachymaran according to claim 1, after it is characterized in that building-up reactions stops, filter, filtrate is decoloured through hydrogen peroxide, its processing condition are: reaction solution and hydrogen peroxide volume ratio are 1000: 1, and normal temperature is more than 10 hours.
3, the novel industrialized production technique of carboxymethylpachymaran according to claim 2, it is characterized in that reaction solution is after decolouring, be neutralized to pH value 6.5～7.5 with hydrochloric acid, the gained neutralizer is behind electrodialysis desalination, carry out drying with spray-dryer, drying temperature is controlled at 103～105 ℃, gets white powder after the drying, and packing is dispatched from the factory.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100535482A CN101407555A (en) | 2007-10-13 | 2007-10-13 | Novel industrialized production technique of carboxymethyl pachyman |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100535482A CN101407555A (en) | 2007-10-13 | 2007-10-13 | Novel industrialized production technique of carboxymethyl pachyman |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101407555A true CN101407555A (en) | 2009-04-15 |
Family
ID=40570780
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100535482A Pending CN101407555A (en) | 2007-10-13 | 2007-10-13 | Novel industrialized production technique of carboxymethyl pachyman |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101407555A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102204936A (en) * | 2011-05-25 | 2011-10-05 | 武汉回盛生物科技有限公司 | Preparation method of total triterpene extract from poria cocos |
| CN102898533A (en) * | 2012-10-08 | 2013-01-30 | 湖北省宏源药业有限公司 | Preparation method of carboxymethyl pachymaran |
| CN103910806A (en) * | 2013-10-22 | 2014-07-09 | 上海海洋大学 | Method for simply preparing crude enteromorpha prolifera polysaccharide |
| CN104302672A (en) * | 2012-02-08 | 2015-01-21 | 伊塔尔麦奇化学股份公司 | Method for the manufacture of concentrated aqueous solutions of alkali metal salt of carboxymethyl fructan |
| CN106008736A (en) * | 2016-06-28 | 2016-10-12 | 陈勇 | Wide-molecular-weight-distribution carboxymethyl pachymaran, and preparation method and application thereof |
| CN107137250A (en) * | 2017-05-12 | 2017-09-08 | 广州娇漾生物科技有限公司 | A kind of moisturizing anti-ageing face mask containing carboxymethylpachymaran |
| CN109988247A (en) * | 2017-12-29 | 2019-07-09 | 瑞普（天津）生物药业有限公司 | A kind of new preparation process of carboxymethylpachymaran |
| CN110655590A (en) * | 2019-10-22 | 2020-01-07 | 靖州县金茶油科技开发有限责任公司 | Production method of pachyman |
-
2007
- 2007-10-13 CN CNA2007100535482A patent/CN101407555A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102204936A (en) * | 2011-05-25 | 2011-10-05 | 武汉回盛生物科技有限公司 | Preparation method of total triterpene extract from poria cocos |
| CN104302672A (en) * | 2012-02-08 | 2015-01-21 | 伊塔尔麦奇化学股份公司 | Method for the manufacture of concentrated aqueous solutions of alkali metal salt of carboxymethyl fructan |
| CN102898533A (en) * | 2012-10-08 | 2013-01-30 | 湖北省宏源药业有限公司 | Preparation method of carboxymethyl pachymaran |
| CN103910806A (en) * | 2013-10-22 | 2014-07-09 | 上海海洋大学 | Method for simply preparing crude enteromorpha prolifera polysaccharide |
| CN106008736A (en) * | 2016-06-28 | 2016-10-12 | 陈勇 | Wide-molecular-weight-distribution carboxymethyl pachymaran, and preparation method and application thereof |
| CN107137250A (en) * | 2017-05-12 | 2017-09-08 | 广州娇漾生物科技有限公司 | A kind of moisturizing anti-ageing face mask containing carboxymethylpachymaran |
| CN109988247A (en) * | 2017-12-29 | 2019-07-09 | 瑞普（天津）生物药业有限公司 | A kind of new preparation process of carboxymethylpachymaran |
| CN110655590A (en) * | 2019-10-22 | 2020-01-07 | 靖州县金茶油科技开发有限责任公司 | Production method of pachyman |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101407555A (en) | Novel industrialized production technique of carboxymethyl pachyman | |
| CN103755824B (en) | The technique of fucoidin in a kind of Enzymatic Extraction marine alga | |
| CN111647027B (en) | Method for separating and purifying N-acetylglucosamine | |
| CN102174119B (en) | Selenized carrageenan and preparation method thereof | |
| CN101250237B (en) | Non-solvent extraction method of chondroitin sulfate | |
| CN111004827B (en) | Preparation method of xylo-oligosaccharide | |
| CN103755822A (en) | Brasenia schreberi polysaccharide preparation method | |
| CN104593446A (en) | Preparation method of pure xylooligosaccharide powder | |
| CN104861079A (en) | Microwave assisted lentinan extraction equipment and technology | |
| CN106103726A (en) | Separate the method for oligosaccharides from agricultural wastes classification | |
| CN104788584A (en) | New technology for clean production of chitosan and carboxymethyl chitosan by using crustacean shell raw materials | |
| CN103382493A (en) | Method for fast producing high-purity mannan-oligosaccharide | |
| CN103450256B (en) | Comprehensive utilization method of defatted rice bran | |
| WO2021248697A1 (en) | Glucosamine salt produced by means of enzymatic method, and purification method therefor | |
| WO2016145977A1 (en) | Enzymatic gelatin preparation process | |
| JP3371124B2 (en) | Acetyl fucoidan from cultured Okinawa mozuku and its production | |
| CN103588892B (en) | A kind of solvent extraction process of wheat bran active polysaccharide | |
| CN107698696B (en) | Preparation method of cassava polyferose | |
| CN106434796A (en) | Method for preparing glycosylated hesperidin | |
| CN101095454A (en) | Method of separating protein from cereal kernel by adopting membrane separation technique | |
| CN103214113B (en) | Chromatographic separation method of sodium chloride and sodium glycollate in waste water in production process of sodium carboxy methyl cellulose | |
| CN102417452A (en) | Preparation method of citrate | |
| CN204752588U (en) | Microwave -assisted draws lentinan's equipment | |
| CN105384836A (en) | Method for improving extraction leaching rate of medicinal and edible fungus beta-glucan | |
| CN104744525A (en) | Process of preparing high-purity L-arabinose by taking Arabic gum as raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090415 |