CN105801719B - A kind of preparation technology of water soluble algae acid calcium and barium alginate - Google Patents
A kind of preparation technology of water soluble algae acid calcium and barium alginate Download PDFInfo
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- CN105801719B CN105801719B CN201610160533.5A CN201610160533A CN105801719B CN 105801719 B CN105801719 B CN 105801719B CN 201610160533 A CN201610160533 A CN 201610160533A CN 105801719 B CN105801719 B CN 105801719B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses the preparation technology of a kind of water soluble algae acid calcium and barium alginate.It is characterized in that preparation technology is：Sodium alginate → water dissolving → dilution → filtering → weak acid acidifying → ultrafiltration → water soluble algae acid → plus alkali neutralization → alcohol precipitation → centrifugation → freeze-drying → crushing → water soluble algae acid calcium or barium alginate.The present invention first prepares water soluble algae acid, carboxyl is present in the form of free state in its molecular structure, neutralized reaction prepares water soluble algae acid calcium, barium alginate again, this has overturned calcium alginate, barium alginate water-insoluble, qualitative change, great application study DEVELOPMENT PROSPECT all occur for both physicochemical properties.
Description
Technical field
The present invention relates to the preparation technology of a kind of water soluble algae acid calcium and barium alginate.
Background technology
The general designation of algin system alginate and alginic acid derivative, it is a kind of natural hydrophilic polymer.By kind master
Solubility alga hydrochlorate and the class of water-insoluble alginate two can be divided into.Water-soluble mainly (the sea of the monovalent salt including alginic acid
Mosanom, potassium, ammonium etc.) and part divalent salts (alginic acid magnesium and alginic acid mercury), water is insoluble including most of alginic acid divalent salts,
It common are calcium alginate, barium alginate (manganese, cobalt) and alginic acid trivalent salt (alginic acid aluminium, iron, chromium etc.).
The difference of the dissolution characteristics of alginate directly determines the difference of its application characteristic.Water miscible alginate master
To apply its thickening property, emulsibility, caking property, film forming；And insoluble alginate mainly applies its ion in application
Gelation during conversion.It can realize that insoluble alginate becomes water soluble algae hydrochlorate by certain technological means, come
Its characteristic is enriched, develops more application studies.
The content of the invention
In view of the above-mentioned problems, the invention provides the preparation technology of a kind of water soluble algae acid calcium and barium alginate, pass through
Prepare water soluble algae acid and water soluble algae acid calcium, barium alginate are prepared by neutralization reaction again.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of preparation technology of water soluble algae acid calcium and barium alginate.It is characterized in that comprise the steps of：
(1) 1% glue is prepared：The glue for taking sodium alginate powder to add water stirring and dissolving into 1%；
(2) dilute：Glue continues to be diluted with water 10~15 times；
(3) filter：The glue diluted crosses 320 eye mesh screens, goes the removal of impurity；
(4) weak acid is acidified：Appropriate weak acid is added in batches in the glue after filtering, starts agitator and stir to reaction
Completely；
(5) ultrafiltration：React complete glue and hyperfiltration treatment is carried out by continous way plate-type hyperfiltration device, go in removing glue liquid
Inorganic salts small molecule, remaining concentrate are water soluble algae acid solution；
(6) neutralize：Appropriate alkali is added into above-mentioned alginic acid solution and carries out neutralization reaction, by the pH for determining reaction solution
Determine reaction end；
(7) alcohol precipitation：After the completion of neutralization, using 1.5~2 times of 95% ethanol precipitation neutralized reaction product；
(8) centrifuge：Alcohol precipitation mixture is injected in centrifuge, moisture removal is removed in centrifugation；
(9) it is freeze-dried：Processing is dried using Freeze Drying Technique in centrifugation product；
(10) dried material granularity needed for pulverizer crushes.
To the further improvement of above-mentioned technical proposal：Glue after step (2) dilution is in 20 DEG C, the rotation of 1% concentration
Viscosity is 5~10mPa.s.
To the further improvement of above-mentioned technical proposal：Weak acid in the step (4) is acetic acid or one kind in phosphoric acid or two
Kind.
To the further improvement of above-mentioned technical proposal：The operating pressure of ultrafiltration apparatus is 0.3MPa, worked in the step (5)
40 DEG C of temperature.
To the further improvement of above-mentioned technical proposal：Alkali in the step (6) is calcium hydroxide or barium hydroxide.
To the further improvement of above-mentioned technical proposal：Moisture≤15% of material after step (9) freeze-drying.
Compared with prior art, the advantages and positive effects of the present invention are：
The present invention first prepares water soluble algae acid, carboxyl is present in the form of free state in its molecular structure, then passes through
Water soluble algae acid calcium, barium alginate are prepared with reaction, this has overturned calcium alginate, barium alginate water-insoluble, both reasons
Change property and qualitative change, great application study DEVELOPMENT PROSPECT all occurs.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of a kind of water soluble algae acid calcium provided by the invention and barium alginate.
Specific embodiment
Embodiment 1
1st, water soluble algae acid calcium production technology, step specially as described below：
(1) 1% glue is prepared：75Kg sodium alginate powders are taken, are added in the agitator tank for filling 7500L volume of water, are stirred
To being completely dissolved, 1% glue of sodium alginate is obtained；
(2) dilute：The above-mentioned glue prepared adds water to continue to be diluted with water 10 times, determines the rotary viscosity of its 1% glue
For 10mPa.s；
(3) filter：The eye mesh screen of glue 320 diluted, goes the removal of impurity；
(4) weak acid is acidified：By appropriate acetic acid it is secondary in three batches be added in the glue of filtering, add during start stirring
Device stirs, and judges final reaction end by detecting reaction solution pH；
(5) ultrafiltration：It is acidified complete reaction solution and hyperfiltration treatment is carried out by continous way plate-type hyperfiltration device, goes in removing glue liquid
Inorganic salts small molecule, remaining concentrate is water soluble algae acid solution, the wherein operating pressure 0.3MPa of ultrafiltration apparatus,
40 DEG C of temperature；
(6) neutralize：Appropriate calcium hydroxide is added into above-mentioned alginic acid solution and carries out neutralization reaction, is reacted by determining
The pH of liquid determines reaction end；
(7) alcohol precipitation：After the completion of neutralization, using 1.5 times of 95% ethanol precipitation neutralized reaction product；
(8) centrifuge：Alcohol precipitation mixture is injected in centrifuge, moisture removal is removed in centrifugation；
(9) it is freeze-dried：Processing is dried using Freeze Drying Technique in centrifugation product；
(10) dried material granularity needed for pulverizer crushes, the water soluble algae acid calcium finally made.
2nd, the water soluble algae acid calcium moisture that after testing prepared by above-mentioned technique is 13.88%, meets standard regulation.
Implementation column 2
1st, water soluble algae acid barium production technology, step specially as described below：
(1) 1% glue is prepared：50Kg sodium alginate powders are taken, are added in the agitator tank for filling 5000L volume of water, are stirred
To being completely dissolved, 1% glue of sodium alginate is obtained；
(2) dilute：The above-mentioned glue prepared adds water to continue to be diluted with water 15 times, determines the rotary viscosity of its 1% glue
For 5mPa.s；
(3) filter：The eye mesh screen of glue 320 diluted, goes the removal of impurity；
(4) weak acid is acidified：By appropriate phosphoric acid it is secondary in three batches be added in the glue of filtering, add during start stirring
Device stirs, and judges final reaction end by detecting reaction solution pH；
(5) ultrafiltration：It is acidified complete reaction solution and hyperfiltration treatment is carried out by continous way plate-type hyperfiltration device, goes in removing glue liquid
Inorganic salts small molecule, remaining concentrate is water soluble algae acid solution, the wherein operating pressure 0.3MPa of ultrafiltration apparatus,
40 DEG C of temperature；
(6) neutralize：Appropriate barium hydroxide is added into above-mentioned alginic acid solution and carries out neutralization reaction, is reacted by determining
The pH of liquid determines reaction end；
(7) alcohol precipitation：After the completion of neutralization, using 2 times of 95% ethanol precipitation neutralized reaction product；
(8) centrifuge：Alcohol precipitation mixture is injected in centrifuge, moisture removal is removed in centrifugation；
(9) it is freeze-dried：Processing is dried using Freeze Drying Technique in centrifugation product；
(10) dried material granularity needed for pulverizer crushes, the water soluble algae acid barium finally made.
2nd, the water soluble algae acid barium moisture that after testing prepared by above-mentioned technique is 14.36%, meets standard regulation.
Embodiment 3
1st, water soluble algae acid calcium production technology, step specially as described below：
(1) 1% glue is prepared：50Kg sodium alginate powders are taken, are added in the agitator tank for filling 5000L volume of water, are stirred
To being completely dissolved, 1% glue of sodium alginate is obtained；
(2) dilute：The above-mentioned glue prepared adds water to continue to be diluted with water 12 times, determines the rotary viscosity of its 1% glue
For 7.5mPa.s；
(3) filter：The eye mesh screen of glue 320 diluted, goes the removal of impurity；
(4) weak acid is acidified：By appropriate acetic acid and phosphoric acid it is secondary in three batches be added in the glue of filtering, add during open
Dynamic agitator stirring, judges final reaction end by detecting reaction solution pH；
(5) ultrafiltration：It is acidified complete reaction solution and hyperfiltration treatment is carried out by continous way plate-type hyperfiltration device, goes in removing glue liquid
Inorganic salts small molecule, remaining concentrate is water soluble algae acid solution, the wherein operating pressure 0.3MPa of ultrafiltration apparatus,
40 DEG C of temperature；
(6) neutralize：Appropriate calcium hydroxide is added into above-mentioned alginic acid solution and carries out neutralization reaction, is reacted by determining
The pH of liquid determines reaction end；
(7) alcohol precipitation：After the completion of neutralization, using 1.8 times of 95% ethanol precipitation neutralized reaction product；
(8) centrifuge：Alcohol precipitation mixture is injected in centrifuge, moisture removal is removed in centrifugation；
(9) it is freeze-dried：Processing is dried using Freeze Drying Technique in centrifugation product；
(10) dried material granularity needed for pulverizer crushes, the water soluble algae acid calcium finally made.
2nd, the water soluble algae acid calcium moisture that after testing prepared by above-mentioned technique is 13.93%, meets standard regulation.
Claims (5)
1. the preparation technology of a kind of water soluble algae acid calcium and barium alginate, is comprised the following steps
(1) 1% glue is prepared：The glue for taking sodium alginate powder to add water stirring and dissolving into 1%；
(2) dilute：Glue continues to be diluted with water 10~15 times；
(3) filter：The glue diluted crosses 320 eye mesh screens, goes the removal of impurity；
(4) weak acid is acidified：Appropriate weak acid is added in batches in the glue after filtering, starts agitator and stir to having reacted
Entirely；
(5) ultrafiltration：React complete glue and hyperfiltration treatment is carried out by continous way plate-type hyperfiltration device, go inorganic in removing glue liquid
Salt small molecule, remaining concentrate are water soluble algae acid solution；
(6) neutralize：Appropriate alkali is added into above-mentioned alginic acid solution and carries out neutralization reaction, wherein alkali is calcium hydroxide or hydrogen-oxygen
Change barium, reaction end is determined by the pH for determining reaction solution；
(7) alcohol precipitation：After the completion of neutralization, using 1.5~2 times of 95% ethanol precipitation neutralized reaction product；
(8) centrifuge：Alcohol precipitation mixture is injected in centrifuge, moisture removal is removed in centrifugation；
(9) it is freeze-dried：Processing is dried using Freeze Drying Technique in centrifugation product；
(10) dried material granularity needed for pulverizer crushes.
2. the preparation technology of a kind of water soluble algae acid calcium according to claim 1 and barium alginate, step described in its feature
Suddenly the glue after (2) dilution is 5~10mPa.s in the rotary viscosity of 20 DEG C, 1% concentration.
3. the preparation technology of a kind of water soluble algae acid calcium according to claim 1 and barium alginate, step described in its feature
Suddenly the weak acid in (4) is one or both of acetic acid or phosphoric acid.
4. the preparation technology of a kind of water soluble algae acid calcium according to claim 1 and barium alginate, step described in its feature
Suddenly the operating pressure of ultrafiltration apparatus is 0.3MPa, 40 DEG C of operating temperature in (5).
5. the preparation technology of a kind of water soluble algae acid calcium according to claim 1 and barium alginate, step described in feature
(9) moisture≤15% of material after being freeze-dried.
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| CN201610160533.5A CN105801719B (en) | 2016-03-21 | 2016-03-21 | A kind of preparation technology of water soluble algae acid calcium and barium alginate |
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| CN201610160533.5A CN105801719B (en) | 2016-03-21 | 2016-03-21 | A kind of preparation technology of water soluble algae acid calcium and barium alginate |
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| CN105801719B true CN105801719B (en) | 2018-01-26 |
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| CN110862561B (en) * | 2019-11-19 | 2022-11-11 | 青岛明月藻酸盐组织工程材料有限公司 | Preparation method of water-insoluble alginate for in vivo implantation |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012286A (en) * | 2006-11-23 | 2007-08-08 | 郑婵颖 | Process for producing water soluble seaweed powder |
| CN101585890A (en) * | 2008-06-20 | 2009-11-25 | 青岛聚大洋海藻工业有限公司 | Method for preparing sodium alginate from kelp |
| CN102977224A (en) * | 2012-12-21 | 2013-03-20 | 青岛明月海藻集团有限公司 | Method for preparing calcium alginate |
| CN103351440A (en) * | 2013-07-31 | 2013-10-16 | 青岛海之林生物科技开发有限公司 | Production technology of pharmaceutical grade sodium alginate |
| CN105111329A (en) * | 2015-09-15 | 2015-12-02 | 常州市鼎日环保科技有限公司 | Method for preparing calcium alginate |
-
2016
- 2016-03-21 CN CN201610160533.5A patent/CN105801719B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012286A (en) * | 2006-11-23 | 2007-08-08 | 郑婵颖 | Process for producing water soluble seaweed powder |
| CN101585890A (en) * | 2008-06-20 | 2009-11-25 | 青岛聚大洋海藻工业有限公司 | Method for preparing sodium alginate from kelp |
| CN102977224A (en) * | 2012-12-21 | 2013-03-20 | 青岛明月海藻集团有限公司 | Method for preparing calcium alginate |
| CN103351440A (en) * | 2013-07-31 | 2013-10-16 | 青岛海之林生物科技开发有限公司 | Production technology of pharmaceutical grade sodium alginate |
| CN105111329A (en) * | 2015-09-15 | 2015-12-02 | 常州市鼎日环保科技有限公司 | Method for preparing calcium alginate |
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Denomination of invention: Preparation of water soluble calcium alginate and barium alginate Effective date of registration: 20200821 Granted publication date: 20180126 Pledgee: Qingdao high tech Cci Capital Ltd. Pledgor: QINGDAO HYZLIN BIOLOGY DEVELOPMENT Co.,Ltd. Registration number: Y2020990001005 |
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Date of cancellation: 20211008 Granted publication date: 20180126 Pledgee: Qingdao high tech Cci Capital Ltd. Pledgor: QINGDAO HYZLIN BIOLOGY DEVELOPMENT Co.,Ltd. Registration number: Y2020990001005 |