CN109666084A - A kind of cleanly production technique of high viscosity sodium alginate - Google Patents
A kind of cleanly production technique of high viscosity sodium alginate Download PDFInfo
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- CN109666084A CN109666084A CN201811609954.7A CN201811609954A CN109666084A CN 109666084 A CN109666084 A CN 109666084A CN 201811609954 A CN201811609954 A CN 201811609954A CN 109666084 A CN109666084 A CN 109666084A
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- sodium alginate
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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
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- 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 present invention is for the problems in existing sodium alginate extraction process, provide a kind of new process of sodium alginate extraction from brown alga, including the immersion of dry brown alga, compound biological enzyme enzymatic hydrolysis, calcification, reverse washing, acidification, neutralization, squeezing, centrifugation, drying and other steps.The cleanly production is eliminated the huge digestion of water consumption in traditional handicraft and rushes dilute step, water resource is greatly saved, production cost is reduced using whole fibrosis production method.Using reverse washing process, industrial water has been saved again.In addition, due to the non-through a long time alkali digestion processing of this technique, the prototype structure length of sodium alginate polysaccharide segment is maintained from the root, therefore the sodium alginate viscosity height and viscosity stability produced are good, stable high viscosity can be kept in high temperature summer, range of viscosities is about in 1500-2000mpa.s.
Description
Technical field
The invention belongs to marine chemical industry product preparation technical fields, and in particular to a kind of high viscosity sodium alginate cleans
Production technology.
Background technique
In brown alga plant, alginic acid is mainly present in brown alga cell wall in the form of sodium salt, calcium salt and a small amount of magnesium salts,
Calcium salt is not soluble in water, but sodium salt is dissolved in water.From seaweed when sodium alginate extraction, it is important to by the various seas in brown alga cell wall
Alginates are converted into sodium alginate and purify out.
Since commercially producing since the nineteen twenty-nine sodium alginate, countries in the world production sodium alginate is substantially all made of pure
Alkali digestion technique makes the alginate in seaweed be converted into sol form sodium alginate and is dissolved in the water, then uses calcium with lye
Salt purifies seaweed acid group, is acidified again later as alginic acid, finally in alcohol in caustic soda and obtaining the alginic acid of high-purity
Sodium.This traditional handicraft process is many and diverse, and soda ash digestion process will consume a large amount of alkali, it is subsequent closely follow rush dilute technique and can expend pole
A large amount of water.100-150 times that dilute process water consumption is about dry brown alga is rushed, the water consumption for producing 1 ton of sodium alginate finished product is caused
Amount is about 700 tons, and water consumption is huge.Process modification how to be carried out to achieve the purpose that water conservation, becomes the industry urgently
It solves the problems, such as.
Sodium alginate plays thickening, emulsification as natural edible colloid, is widely used in food every profession and trade.It is existing
The sodium alginate viscosity stability of technique production is poor, and nature decline can be occurred by placing a period of time viscosity, especially in sweltering heat
Summer, viscosity decline are more rapid.Aiming at the problem that high viscosity sodium alginate is difficult to prepare, domestic and foreign scholars have been carried out largely
Experimental study.
A kind of method for improving sodium alginate viscosity and stability of patent CN101942121A, technique essentially will
PEG600 solution is added in activation sodium alginate soln, is reacted, and carries out ultrafiltration, concentration using film after reaction, most
The sodium alginate that viscosity is higher, stability is good is made in solution freeze-drying again afterwards.Wherein PEG600 is a kind of bonding well
Agent.This method improves the viscosity of sodium alginate by means of the cementation of PEG600, but the introducing of PEG600 cannot be gone at all
It removes, so that product is impure, furthermore this method carries out ultrafiltration using film, and compared with actual production, the introducing of film, which will increase, to be produced into
This, is not suitable for carrying out scale industrial production.
A kind of preparation method of high-viscosity alginate of patent CN102492053A, technique are brown alga digestion preparation seaweed
The calcium carbonate of alginic acid obtained and 0.5%-3% is added in neutralization reactor by acid, solid phase neutralization reaction 10-20min mesh
Be that alginic acid is first made to be converted to calcium alginate on a small quantity, the alginic acid after reaction adds alkali neutralization to being fully converted into algin.This
Method uses solid phase transformation, introduces exogenous material calcium carbonate, and a small amount of calcium alginate of generation is first reacted with alginic acid and is carried out again
It neutralizes complete.
A kind of production technology of hyperviscosity algin of patent CN1048041108A, technique are alginic acid and alginic acid
Calcium carries out neutralization reaction after arranging in pairs or groups according to different ratio, and high-viscosity alginate is made.The algin product of the method production, calcic
Amount is high, therefore has high pseudoplastic behavior viscosity, but be unable to satisfy the requirement of low calcium product, and storage medium viscosity declines
Fastly, unstable.
Summary of the invention
The present invention provides a kind of high viscosity sodium alginate cleaning metaplasia for the status of prior art production sodium alginate
The production technology of production.The cleanly production processing step simplifies, and eliminates the big digestion of water consumption in traditional handicraft and rushes dilute step,
Water resource is greatly saved, reduces production cost.In addition, due to the non-through a long time alkali digestion processing of this technique, from the root
The prototype structure length of sodium alginate polysaccharide segment is maintained, therefore the sodium alginate viscosity produced is high and viscosity stability is good,
Stable high viscosity can be kept in high temperature summer, range of viscosities is about in 1500-2000mpa.s.
The present invention is the high-valued development and utilization to sodium alginate production technology, simplifies sodium alginate production technology.
For achieving the above object, the present invention, which adopts the following technical solutions, is achieved:
A kind of cleanly production technique of high viscosity sodium alginate, the described method comprises the following steps:
(1) dry brown alga is impregnated: brown alga is put into abundant rehydration in enzymatic vessel, amount of water is about 8-10 times, rehydration time:
6-8h；
(2) complex enzyme zymohydrolysis: enzymatic vessel temperature is adjusted to 40-55 degrees Celsius, pH 4.5-5.5, and complex enzyme (egg is added
White enzyme: cellulase: pectase=1:1:1.2-1.5), additional amount is dry brown alga weight 1-3%, enzyme digestion reaction 3-5h, purpose
It is to decompose albumen, pectin, cellulose etc. in brown alga completely；
(3) calcification: calcium chloride being added into enzymatic vessel, until calcium chloride concentration is 5% or so, fills seaweed acid group therein
Divide calcification, is converted into fibrous calcium alginate；
(4) reverse washing: calcium alginate fibre is transported to a high position with conveyer belt, connects water jet to alginate fibre in high level
Into back flush.Water washes the impurity such as the pectin digested and fiber, and filtered cleaning solution can be used as impregnating dry brown alga
Soak, residue is for making alga fertilizer；
(5) it squeezes: calcium alginate fibre being subjected to press dewatering with twin rollers；
(6) it is acidified: dewatered calcium alginate fibre being put into souring tank by conveyer belt, is acidified with hydrochloric acid, salt
The Baume angle value of acid is 6-7 ° of B é, obtains alginic acid fibre；
(7) squeeze: with the moisture in screw press and hydraulic press removal alginic acid, moisture is below 70% after squeezing；
(8) alcohol neutralizes: using alcohol as medium, alginic acid is reacted with sodium hydroxide solution generates sodium alginate, neutralizes anti-
Control judges reaction end in 40~50min with universal indicator chromogenic reaction between seasonable；
(9) it is centrifuged: carrying out centrifugal treating to reacting rear material is neutralized with flat centrifuge, remove moisture, centrifugation time
Control is in 40~45min；
(10) it crushes, obtain high viscosity sodium alginate after drying.
In the step (2), complex enzyme is protease, cellulase and pectase, wherein protease: cellulase: fruit
Glue enzyme=1:1:1.2-1.5；
In the step (4), reverse washing transports calcium alginate fibre using conveyer belt, and conveyer belt parameter is that length is 7-
8 meters, it is in 30 ° of angles with ground, can facilitates and calcium alginate fibre is risen into a high position, is accessed at the rear (at 3.5-4 rice) of conveyer belt
Multiple water jets repeatedly carry out spraying-rinsing processing to calcium alginate on a small quantity.This mode is conducive to improve flush efficiency and water-saving.
The present invention improves in terms of having following four compared with current sodium alginate production technology:
(1) complex enzyme zymohydrolysis brown alga removes the other structures ingredient other than algal polysaccharide by complex enzyme hydrolysis mode, improves
Reaction efficiency, saves the reaction time, has saved water consumption；
(2) direct calcification after digesting, and process (sol form process) is digested without tradition, realize full technical process
Fibrosis production, simplifies production process, reduces the dosage of chemicals, protect polysaccharide structures from the root, ensure that
The high viscosity of sodium alginate；
(3) reverse washing process is used, a small amount of repeatedly washing is significantly more efficient to remove the impurity taken off in calcification process,
It ensure that product purity；
(4) dilute technical process is rushed without tradition, substantially reduces water consumption, and water scouring water is Ke Xunhuanliyong after calcification,
Realize the production of high-efficiency cleaning metaplasia.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
(1) dry brown alga is impregnated: brown alga being put into abundant rehydration in enzymatic vessel, amount of water is about 8 times, rehydration time: 6h；
(2) complex enzyme zymohydrolysis: enzymatic vessel temperature is adjusted to 40 DEG C, pH 4.5, and complex enzyme (protease: cellulose is added
Enzyme: pectase=1:1:1.2), additional amount is dry brown alga weight 1%, enzyme digestion reaction 3h, it is therefore an objective to by albumen in brown alga, pectin,
Cellulose etc. decomposes completely；
(3) calcification: calcium chloride being added into enzymatic vessel, until calcium chloride concentration is 5%, makes the abundant calcium of seaweed acid group therein
Change, is converted into fibrous calcium alginate；
(4) reverse washing: calcium alginate fibre is transported to a high position with conveyer belt, connects water jet to alginate fibre in high level
Into back flush.Water washes the impurity such as the pectin digested and fiber, and filtered cleaning solution can be used as impregnating dry brown alga
Soak, residue is for making alga fertilizer；
(5) it squeezes: calcium alginate fibre being subjected to press dewatering with twin rollers；
(6) it is acidified: dewatered calcium alginate fibre being put into souring tank by conveyer belt, is acidified with hydrochloric acid, salt
The Baume angle value of acid is 6 ° of B é, obtains alginic acid fibre；
(7) squeeze: with the moisture in screw press and hydraulic press removal alginic acid, moisture is 68% after squeezing.
(8) alcohol neutralizes: using alcohol as medium, alginic acid is reacted with sodium hydroxide solution generates sodium alginate, neutralizes anti-
Control judges reaction end in 30min with universal indicator chromogenic reaction between seasonable；
(9) it is centrifuged: carrying out centrifugal treating to reacting rear material is neutralized with flat centrifuge, remove moisture, centrifugation time
Control is in 40min；
(10) it crushes, obtain high viscosity sodium alginate after drying, the viscosity through laboratory detection sodium alginate is
2000mpa.s。
Embodiment 2
(1) dry brown alga is impregnated: brown alga being put into abundant rehydration in enzymatic vessel, amount of water is about 9 times, rehydration time: 7h；
(2) complex enzyme zymohydrolysis: enzymatic vessel temperature is adjusted to 45 DEG C, pH 5.0, and complex enzyme (protease: cellulose is added
Enzyme: pectase=1:1:1.3), additional amount is dry brown alga weight 2%, enzyme digestion reaction 4h, it is therefore an objective to by albumen in brown alga, pectin,
Cellulose etc. decomposes completely；
(3) calcification: calcium chloride being added into enzymatic vessel, until calcium chloride concentration is 5%, makes the abundant calcium of seaweed acid group therein
Change, is converted into fibrous calcium alginate；
(4) reverse washing: calcium alginate fibre is transported to a high position with conveyer belt, connects water jet to alginate fibre in high level
Into back flush.Water washes the impurity such as the pectin digested and fiber, and filtered cleaning solution can be used as impregnating dry brown alga
Soak, residue is for making alga fertilizer；
(5) it squeezes: calcium alginate fibre being subjected to press dewatering with twin rollers；
(6) it is acidified: dewatered calcium alginate fibre being put into souring tank by conveyer belt, is acidified with hydrochloric acid, salt
The Baume angle value of acid is 6.5 ° of B é, obtains alginic acid fibre；
(7) squeeze: with the moisture in screw press and hydraulic press removal alginic acid, moisture is 67% after squeezing.
(8) alcohol neutralizes: using alcohol as medium, alginic acid is reacted with sodium hydroxide solution generates sodium alginate, neutralizes anti-
Control judges reaction end in 40min with universal indicator chromogenic reaction between seasonable；
(9) it is centrifuged: carrying out centrifugal treating to reacting rear material is neutralized with flat centrifuge, remove moisture, centrifugation time
Control is in 45min；
(10) it crushes, obtain high viscosity sodium alginate after drying, the viscosity through laboratory detection sodium alginate is
1700mpa.s。
Embodiment 3
(1) dry brown alga is impregnated: brown alga is put into abundant rehydration in enzymatic vessel, amount of water is about 10 times, rehydration time:
8h；
(2) complex enzyme zymohydrolysis: enzymatic vessel temperature is adjusted to 55 DEG C, pH 5.5, and complex enzyme (protease: cellulose is added
Enzyme: pectase=1:1:1.5), additional amount is dry brown alga weight 3%, enzyme digestion reaction 5h, it is therefore an objective to by albumen in brown alga, pectin,
Cellulose etc. decomposes completely；
(3) calcification: calcium chloride being added into enzymatic vessel, until calcium chloride concentration is 5%, makes the abundant calcium of seaweed acid group therein
Change, is converted into fibrous calcium alginate；
(4) reverse washing: calcium alginate fibre is transported to a high position with conveyer belt, connects water jet to alginate fibre in high level
Carry out back flush.Water washes the impurity such as the pectin digested and fiber, and filtered cleaning solution can be used as impregnating dry brown alga
Soak, residue is for making alga fertilizer；
(5) it squeezes: calcium alginate fibre being subjected to press dewatering with twin rollers；
(6) it is acidified: dewatered calcium alginate fibre being put into souring tank by conveyer belt, is acidified with hydrochloric acid, salt
The Baume angle value of acid is 7 ° of B é, obtains alginic acid fibre；
(7) squeeze: with the moisture in screw press and hydraulic press removal alginic acid, moisture is 65% after squeezing；
(8) alcohol neutralizes: using alcohol as medium, alginic acid is reacted with sodium hydroxide solution generates sodium alginate, neutralizes anti-
Control judges reaction end in 45min with universal indicator chromogenic reaction between seasonable；
(9) it is centrifuged: carrying out centrifugal treating to reacting rear material is neutralized with flat centrifuge, remove moisture, centrifugation time
Control is in 50min；
(10) it crushes, obtain high viscosity sodium alginate after drying, the viscosity through laboratory detection sodium alginate is
1500mpa.s。
Claims (5)
1. a kind of cleanly production technique of high viscosity sodium alginate, comprising the following steps:
(1) dry brown alga is impregnated: brown alga being put into abundant rehydration in enzymatic vessel, amount of water is about 8-10 times, rehydration time: 2-
8h；
(2) complex enzyme zymohydrolysis: enzymatic vessel temperature is adjusted to 40-55 DEG C, pH 4.5-5.5, addition complex enzyme (cellulase:
Pectase=1:1.2-1.5), additional amount is dry brown alga weight 1-3%, enzyme digestion reaction 3-5h, it is therefore an objective to by pectin, fibre in brown alga
Element etc. is tieed up to decompose completely；
(3) calcification: calcium chloride being added into enzymatic vessel, until calcium chloride concentration is 5% or so, makes the abundant calcium of seaweed acid group therein
Change, is converted into fibrous calcium alginate；
(4) reverse washing: with being in 30 ° of angles with ground, length is that calcium alginate fibre is risen to a high position by 7-8 meters of conveyer belt,
Multiple water jets are accessed at the rear (at 3.5-4 meters) of conveyer belt, repeatedly carry out spraying-rinsing processing to calcium alginate on a small quantity.Use water
The impurity such as the pectin digested and fiber are washed, filtered cleaning solution can be used as impregnating the soak of dry brown alga, and residue is used
In production alga fertilizer；
(5) it squeezes: calcium alginate fibre being subjected to press dewatering with twin rollers；
(6) it is acidified: dewatered calcium alginate fibre being put into souring tank by conveyer belt, is acidified with hydrochloric acid, hydrochloric acid
Baume angle value is 6-7 Baume degrees, obtains alginic acid fibre；
(7) squeeze: with the moisture in screw press and hydraulic press removal alginic acid, moisture is below 70% after squeezing；
(8) alcohol neutralizes: using alcohol as medium, alginic acid reacts generation sodium alginate with sodium hydroxide solution, when neutralization reaction
Between control in 40~60min, reaction end is judged with universal indicator chromogenic reaction；
(9) it is centrifuged: carrying out centrifugal treating to reacting rear material is neutralized with flat centrifuge, remove moisture, centrifugation time control
In 40~45min；
(10) it crushes, obtain high viscosity sodium alginate after drying.
2. a kind of cleanly production technique of high viscosity sodium alginate according to claim 1, it is characterised in that: the step
Suddenly in (2), complex enzyme is protease, cellulase and pectase, wherein protease: cellulase: pectase=1:1:1.2-
1.5。
3. a kind of cleanly production technique of high viscosity sodium alginate according to claim 1, it is characterised in that: the step
Suddenly in (4), reverse washing transports calcium alginate fibre using conveyer belt, and conveyer belt parameter is that length is 7-8 meters, is in ground
30 ° of angles, can facilitate calcium alginate fibre rising to a high position, access multiple water jets at the rear (at 3.5-4 rice) of conveyer belt, few
Amount repeatedly carries out spraying-rinsing processing to calcium alginate.
4. a kind of cleanly production technique of high viscosity sodium alginate according to claim 1, it is characterised in that: the step
Suddenly in (6), the alcoholic strength of neutralization alcohol is 60-85 °, and the Baume degrees of neutralization sodium hydroxide solution is 20-30 Baume degrees.
5. a kind of cleanly production technique of high viscosity sodium alginate according to claim 1, it is characterised in that: entire raw
Production. art process product realizes whole fibrosis, and no glue state existence form belongs to realization and cleans the new of water-saving production
Method.
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Application publication date: 20190423 |
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| RJ01 | Rejection of invention patent application after publication |