CN102190816B - Marine polysaccharide and manufacturing process thereof - Google Patents

Marine polysaccharide and manufacturing process thereof Download PDF

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Publication number
CN102190816B
CN102190816B CN 201110080776 CN201110080776A CN102190816B CN 102190816 B CN102190816 B CN 102190816B CN 201110080776 CN201110080776 CN 201110080776 CN 201110080776 A CN201110080776 A CN 201110080776A CN 102190816 B CN102190816 B CN 102190816B
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raw material
raw materials
washing
saccharan
water
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CN102190816A (en
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刘京花
王红梅
杨晓桐
孙明
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Shandong Lefeng Biotechnology Co ltd
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山东乐丰生物科技有限公司
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Abstract

The invention, which relates to a marine polysaccharide and its manufacturing process, pertains to the technical field of marine biomacromolecule polymers. The raw materials formula comprises 30-70 wt% of shrimp shell or crab shell or shrimp shell and crab shell and 30-70 wt% of one or more materials selected from the group consisting of sea-tangle, Eucheuma, asparagus and kelp. The manufacturing process provided by the invention comprises the following steps of: (1) preparing clean raw materials; (2) carrying out an alkali treatment on the raw materials by using a NaOH solution; (3) washing the raw materials to remove the alkali lye; (4) processing the washed raw materials by using a mixed liquor of HCL and H2SO4; (5) washing the raw materials to remove the acid solution; (6) digesting and dissolving the raw materials by using a mixed liquor of protease and cellulase; (7) carrying out the insulation pressure filtration on the dissolved substances to produce a filtrate; (8) solidifying and maturing the filtrate by using a mixed liquor of KCL and CaCL2; (9) dehydrating the matured solid; (10) crushing the bulk solid into particles by using a pulverizer; (11) drying the particles; and (12) sterilizing the dried particles to obtain the marine polysaccharide product. The manufacturing process provided by the invention is scientific and reasonable. The marine polysaccharide product is easy to dissolve, has strong water retention, adjustable viscosity and adjustable gel strength.

Description

A kind of ocean saccharan and production technique thereof
One, technical field
The present invention relates to a kind of ocean saccharan polymer novel material and production technique thereof, belong to marine organisms high molecular polymer and technical field of producing thereof.
Two, background technology
In the existing marine organisms goods relative merits are arranged respectively, can not satisfy simultaneously the several functions needs.Bad such as the chitin solvability, can only be dissolved in organic solvent; Chitosan is water-soluble, but water-retentivity descends and soltion viscosity is bad; Sodium alginate is water-soluble, and viscosity is good, but gel-strength is low, poor water retention property; Carrageenin, agar gel intensity are good, but water insoluble under the normal temperature.More than five kinds of product shortcomings: can not satisfy simultaneously soluble, good water-retaining property, intensity is high behind the gel, intensity is arranged after the film forming, soltion viscosity is high, and also mutability is water insoluble, and therefore the use on medicine, makeup, food and agricultural is limited to, cause use cost too high, the phenomenon such as result of use is poor.
Three, summary of the invention
The object of the invention is to solve the deficiency that above-mentioned prior art exists, a kind of ocean saccharan and production technique thereof of superpower water conservation are provided, this novel sea saccharan can overcome the different shortcomings of above five kinds of marine polysaccharides, satisfy simultaneously soluble in water, water-retentivity is strong, viscosity 50-20000MPa.S height is adjustable, gel-strength 20-2800g/cm 2The features such as height is adjustable.
The present invention is achieved by the following technical solutions:
A kind of ocean saccharan, its special character are that raw material comprises following component, are respectively by the mass percent of each component: shrimp shell or crab shell or shrimp shell and crab shell 30-70%, sea-tangle, Eucheuma muricatum (Gmel.) Web. Van Bos., Thallus Gracilariae, bulk kelp any or several 30-70%.
The production technique of above-mentioned ocean saccharan may further comprise the steps:
(1) prepare raw material: remove first various impurity in the raw material, take by weighing various raw materials by the mass percent of each component, raw material drying to moisture is lower than 38%, it is for subsequent use that salt soaks under the condition prolonged preservation.
(2) alkaline purification: with the NaOH solution of raw material with 7-12% concentration, under 55-65 ℃ of condition, soaked 3-4 hour.
(3) washing alkali lye: the raw material water after the alkaline purification steeps first to be washed, and then is flushed to pH value and reaches below 7.5.
(4) acid treatment: with HCL and H 2SO 4By volume (1.8-2.2): 1, be made into mixed solution, then be diluted to pH value 1.5-2, with the raw material soaking after the above-mentioned washing wherein 15-30 minute, treat that raw material is softening to take out at once.
(5) washing acid solution: the raw material water after the acid treatment washes first, and then bubble is washed pH value and reached more than 6.5.
(6) digestion dissolving: in water, add the proteolytic enzyme of quality 2.5-3.5 ‰ under the normal temperature condition, the cellulase of 1.5-2.5 ‰ is made solution, with the raw material soaking of washing after the acid solution wherein 8-12 hour, then be warming up to 110-130 ℃, be incubated 2-3 hour, fully dissolving.
(7) filter: the material after the above-mentioned dissolving is incubated press filtration, and filtration temperature needs during filtration just can pass through smoothly with 30-50 times of volume hot water dilution more than 85 ℃, gets filtered liquid after the filtration.
(8) solidify aging: with KCL, the CaCL of 8-10% of mass percent concentration 5-8% 2With volume ratio (6-8): 1 ratio is made mixed solution, with filtered liquid and mixed solution with (8-12): 1 volume ratio mixing, solidify burin-in process, the time is 1-1.5 hour.
(9) dehydration: the solid that will wear out is pressed the moisture that removes 20-30% through plate type pressure filter, when noticing that the pressure filter high pressure reaches 8MPa pressure, needs step-down to process.
(10) pulverize: the blocks of solid after will dewatering is ground into the particulate material of 2-5mm size with pulverizer.
(11) oven dry: the dryer inlet temperature is lower than 90 ℃, and temperature out is higher than 40 ℃, and particulate material is dried between the moisture 22-26%.
(12) sterilization: Killing germs by microwave, temperature are 70-85 ℃, time 1.5-2 minute, then use 121 ℃ of steam sterilization pans, and sterilized 10-20 minute, obtain ocean saccharan product.
(13) fine powder: pulverize products obtained therefrom with pawl formula fine pulverizer, through the vibratory screening apparatus classification, crushing material is classified as 40 orders, 80 orders, 120 orders.
(14) homogeneous: granularity on request, viscosity, gel-strength, solubleness, water conservation multiple compound go out the qualified product of requirement.
(15) by packing of product requirement, the packing warehouse-in.
The present invention's a kind of ocean saccharan and production technology characteristics and beneficial effect: satisfy soluble in water, water-retentivity is strong, viscosity 50-20000MPa.S height is adjustable, gel-strength 20-2800g/cm 2Height is adjustable.
1, production technique is scientific and reasonable, and the animal-plant material combination treatment is saved artificial, the energy, auxiliary material and water, and production cost declines to a great extent.
2, select the synergy of the common degraded of proteolytic enzyme and cellulase fairly obvious, effective, than single hot water dissolving, reduce energy consumption more than 40%, and can be by ratio and the concentration control of adjusting enzyme.Degradation temperature and time are controlled molecular weight and the polymerization degree of saccharan, thereby reach many performances and the multi-usage of control product.
3, select and mix peptizer and changed concentrated method by dehydration of alcohol, greatly improved feasibility and the economy of ocean saccharan on cost and the safety.
4, after the ocean saccharan was made, this material became tridimensional network, and molecular weight can be controlled between 2000-1200000, therefore good water-retentivity is arranged, between water retention capacity 400-900 times, controlled solubility and insoluble is arranged, higher viscosity is arranged, larger gel-strength is arranged.
Four, embodiment
Below provide the specific embodiment of the present invention, be used for formation of the present invention is further specified.
Embodiment 1
A kind of ocean saccharan of present embodiment, its raw material comprises following component, is respectively by the mass percent of each component: shrimp shell 10%, crab shell 20%, sea-tangle 10%, Eucheuma muricatum (Gmel.) Web. Van Bos. 15%, Thallus Gracilariae 25%, bulk kelp 20%.
The production technique of above-mentioned a kind of ocean saccharan may further comprise the steps:
(1) prepare raw material: remove various impurity in the raw material, take by weighing various raw materials by the mass percent of each component, raw material must not have and goes mouldy, and raw material drying to moisture is lower than 38%, and it is for subsequent use that salt soaks under the condition prolonged preservation.
(2) alkaline purification: with the NaOH solution of raw material with 7-12% concentration, under 55-65 ℃ of condition, soaked 3-4 hour.
(3) washing alkali lye: the raw material water after the alkaline purification steeps first to be washed, and then is flushed to pH value and reaches below 7.5.
(4) acid treatment: with HCL and H 2SO 4By volume (1.8-2.2): 1, be made into mixed solution, then be diluted to pH value 1.5-2, with the raw material soaking wherein 15-30 minute after the washing, treat that raw material is softening to take out at once.
(5) washing acid solution: the raw material water after the acid treatment washes first, and then bubble is washed pH value and reached more than 6.5.
(6) digestion dissolving: in water, add the proteolytic enzyme of quality 2.5-3.5 ‰ under the normal temperature condition, the cellulase of 1.5-2.5 ‰ is made solution, with the raw material soaking of washing after the acid solution wherein 8-12 hour, then be warming up to 110-130 ℃, be incubated 2-3 hour, fully dissolving.
(7) filter: the material after the above-mentioned dissolving is incubated press filtration, during filtration solution temperature 85-99 ℃, need during filtration just can pass through smoothly with 30-50 times of volume hot water dilution, after the filtration filtered liquid.
(8) solidify aging: with KCL, the CaCL of 8-10% of mass percent concentration 5-8% 2With volume ratio (6-8): 1 ratio is made mixed solution, with filtered liquid and mixed solution with (8-12): 1 volume ratio mixing, solidify burin-in process, the time is 1-1.5 hour.
(9) dehydration: the solid that will wear out is pressed the moisture that removes 20-30% through plate type pressure filter, when noticing that the pressure filter high pressure reaches 8MPa pressure, needs step-down to process.
(10) pulverize: the blocks of solid after will dewatering is ground into the particulate material of 2-5mm size with pulverizer.
(11) oven dry: the dryer inlet temperature is controlled at 70-90 ℃, temperature out 40-60 ℃, particulate material is dried between the moisture 22-26%.
(12) sterilization: the Killing germs by microwave temperature is 70-85 ℃, time 1.5-2 minute, then use 121 ℃ of steam sterilization pans, and sterilized 10-20 minute, obtain ocean saccharan product.
(13) fine powder: pulverize products obtained therefrom with pawl formula fine pulverizer, through the vibratory screening apparatus classification, crushing material is classified as 40 orders, 80 orders, 120 orders.
(14) homogeneous: granularity on request, viscosity, gel-strength, solubleness, water conservation multiple compound go out the qualified product of requirement.
(15) by packing of product requirement, the packing warehouse-in.
Embodiment 2
A kind of ocean saccharan of present embodiment, difference from Example 1 is that its raw material comprises following component, is respectively by the mass percent of each component: crab shell 40%, sea-tangle 20%, Thallus Gracilariae 15%, bulk kelp 25%.
Embodiment 3
A kind of ocean saccharan of present embodiment, difference from Example 1 is that its raw material comprises following component, is respectively by the mass percent of each component: shrimp shell 30%, Eucheuma muricatum (Gmel.) Web. Van Bos. 25%, Thallus Gracilariae 35%, bulk kelp 10%.
Embodiment 4
A kind of ocean saccharan of present embodiment, difference from Example 1 is that its raw material comprises following component, is respectively by the mass percent of each component: crab shell 10%, shrimp shell 30%, sea-tangle 20%, Thallus Gracilariae 25%, bulk kelp 15%.
Embodiment 5
A kind of ocean saccharan of present embodiment, difference from Example 1 is that its raw material comprises following component, is respectively by the mass percent of each component: shrimp shell 70%, Eucheuma muricatum (Gmel.) Web. Van Bos. 5%, sea-tangle 15%, bulk kelp 10%.
Embodiment 6
A kind of ocean saccharan of present embodiment, difference from Example 1 is that its raw material comprises following component, is respectively by the mass percent of each component: crab shell 70%, Eucheuma muricatum (Gmel.) Web. Van Bos. 10%, Thallus Gracilariae 15%, sea-tangle 5%.
Following experimental data prove ocean of the present invention saccharan satisfy soluble in water, water-retentivity is strong, viscosity 50-20000MPa.S height is adjustable, gel-strength 20-2800g/cm 2The characteristic that height is adjustable.
Performance Water-soluble Water-retentivity Viscosity MPa.S Gel-strength g/cm 2
Embodiment 1 Yi Rong By force 50 600
Embodiment 2 Yi Rong By force 10000 20
Embodiment 3 Yi Rong By force 20000 2800
Embodiment 4 Yi Rong By force 2000 2000
Embodiment 5 Yi Rong By force 15000 1500
Embodiment 6 Yi Rong By force 6000 1000
The present invention's a kind of ocean saccharan and production technology characteristics and beneficial effect:
1, production technique is scientific and reasonable, and the animal-plant material combination treatment is saved artificial, the energy, auxiliary material and water, and production cost declines to a great extent.
2, select the synergy of the common degraded of proteolytic enzyme and cellulase fairly obvious, effective, than single hot water dissolving, reduce energy consumption more than 40%, and can be by ratio and the concentration control of adjusting enzyme.Degradation temperature and time are controlled molecular weight and the polymerization degree of saccharan, thereby reach many performances and the multi-usage of control product.
3, select and mix peptizer and changed concentrated method by dehydration of alcohol, greatly improved feasibility and the economy of ocean saccharan on cost and the safety.
4, after the ocean saccharan was made, this material became tridimensional network, and molecular weight can be controlled between 2000-1200000, therefore good water-retentivity is arranged, between water retention capacity 400-900 times, controlled solubility and insoluble is arranged, higher viscosity is arranged, larger gel-strength is arranged.
Ocean of the present invention saccharan is through cosmetic industry, food service industry, and experiments such as soil water-retaining, agriculture Controlled Release Fertilizer and agriculture foliage fertilizer, but proves thickening, moulding, water conservation, the controlled release of good natural degradation, the novel purely natural ocean high molecular polymer of film forming.

Claims (1)

1. an ocean saccharan is characterized in that comprising in the raw material following component, is respectively by the mass percent of each component: shrimp shell or crab shell or shrimp shell and crab shell 30-70%, sea-tangle, Eucheuma muricatum (Gmel.) Web. Van Bos., Thallus Gracilariae, bulk kelp any or several 30-70%;
The manufacture method of ocean saccharan may further comprise the steps:
(1) prepare raw material: remove first various impurity in the raw material, take by weighing various raw materials by the mass percent of each component, raw material drying to moisture is lower than 38%, it is for subsequent use that salt soaks under the condition prolonged preservation;
(2) alkaline purification: with the NaOH solution of raw material with 7-12% concentration, under 55-65 ℃ of condition, soaked 3-4 hour;
(3) washing alkali lye: the raw material water after the alkaline purification steeps first to be washed, and then is flushed to the pH value and reaches below 7.5;
(4) acid treatment: with HCl and H 2SO 4By volume (1.8-2.2): 1, be made into mixed solution, then be diluted to pH value 1.5-2, with the raw material soaking after the above-mentioned washing wherein 15-30 minute, treat that raw material is softening to take out at once;
(5) washing acid solution: the raw material water after the acid treatment washes first, and then bubble is washed the pH value and reached more than 6.5;
(6) digestion dissolving: in water, add the proteolytic enzyme of quality 2.5-3.5 ‰ under the normal temperature condition, the cellulase of 1.5-2.5 ‰ is made solution, with the raw material soaking of washing after the acid solution wherein 8-12 hour, then be warming up to 110-130 ℃, be incubated 2-3 hour, treat abundant dissolving;
(7) filter: the material after the above-mentioned dissolving is incubated press filtration, and filtration temperature needs during filtration just can pass through smoothly with 30-50 times of volume hot water dilution more than 85 ℃, gets filtered liquid after the filtration;
(8) solidify aging: with KCl, the CaCl of 8-10% of mass percent concentration 5-8% 2With volume ratio (6-8): 1 ratio is made mixed solution, with filtered liquid and mixed solution with (8-12): 1 volume ratio mixing, solidify burin-in process, the time is 1-1.5 hour;
(9) dehydration: the solid that will wear out is pressed the moisture that removes 20-30% through plate type pressure filter, when noticing that the pressure filter high pressure reaches 8MPa pressure, needs step-down to process;
(10) pulverize: the blocks of solid after will dewatering is ground into the particulate material of 2-5mm size with pulverizer;
(11) oven dry: the dryer inlet temperature is lower than 90 ℃, and temperature out is higher than 40 ℃, and particulate material is dried between the moisture 22-26%;
(12) sterilization: Killing germs by microwave, temperature are 70-85 ℃, time 1.5-2 minute, then use 121 ℃ of steam sterilization pans, and sterilized 10-20 minute, obtain ocean saccharan product.
CN 201110080776 2011-04-01 2011-04-01 Marine polysaccharide and manufacturing process thereof Expired - Fee Related CN102190816B (en)

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Publication number Priority date Publication date Assignee Title
CN102942639A (en) * 2012-12-12 2013-02-27 石狮市华宝海洋生物化工有限公司 Method for improving production purity of chitin
CN109576329B (en) * 2018-12-29 2021-05-18 广东医科大学 Preparation method, product and application of anti-melanin synthesized asparagus non-agar oligosaccharide
CN110028599A (en) * 2019-05-14 2019-07-19 深圳市仙迪化妆品有限公司 A kind of preparation method of algae chitosan

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JPH06254393A (en) * 1993-03-04 1994-09-13 Mitsui Eng & Shipbuild Co Ltd Water retention agent and its production
CN1252954A (en) * 1998-11-06 2000-05-17 荣成市神通海洋生物公司 Process for preparing liquid extract of kelp
DE19920688A1 (en) * 1999-05-05 2000-11-23 Manfred Kuhn Radiolytically modified heteropolysaccharides
CN1166692C (en) * 2000-06-06 2004-09-15 南京大学科技实业(集团)公司 Process for preparing gold element mucopolysaccharide latex
CN1184237C (en) * 2003-01-07 2005-01-12 江南大学 Preparation of crust oligosaccharide and use
CN101134783B (en) * 2007-10-19 2010-06-16 大连工业大学 Method for preparing sea-tangle polysaccharide
CN101451157B (en) * 2008-12-25 2012-09-05 大连海晏堂生物有限公司 Method for preparing low molecular weight sea cucumber polysaccharide

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