阅读说明：本技术 一种Kappa卡拉胶胶液的制备方法 (Preparation method of Kappa carrageenan glue solution ) 是由 肖安风 刘尧 于 2020-05-15 设计创作，主要内容包括：本发明提供一种Kappa卡拉胶胶液的制备方法,其特征在于,包括以下步骤：将K型麒麟菜置于Ca(OH)-(2)溶液环境中；加热化胶；通入CO-(2),以与Ca(OH)-(2)反应生成CaCO-(3)；过滤,获得Kappa卡拉胶胶液。本发明通过Ca(OH)-(2)溶液结合煮胶对K型麒麟菜进行处理,再通过CO-(2)去除Ca(OH)-(2),可制备出高凝胶强度、高产率的Kappa卡拉胶,使卡拉胶具备较高的产品品质。该方法工艺简单,绿色环保,产品生产周期较短,原料安全且来源广,减少了提取过程中水资源的浪费,也避免了提取过程中产生的废液排放,是一种新型的绿色制备方法。(The invention provides a preparation method of Kappa carrageenan glue solution, which is characterized by comprising the following steps: placing K type Eucheuma Gelatinosum in Ca (OH) 2 In a solution environment; heating to melt the glue; introducing CO 2 To react with Ca (OH) 2 Reaction to form CaCO 3 (ii) a Filtering to obtain Kappa carrageenan glue solution. The invention is realized by Ca (OH) 2 Treating Eucheuma K with solution and boiled gelatin, and introducing CO 2 Removal of Ca (OH) 2 The Kappa carrageenan with high gel strength and high yield can be prepared, so that the carrageenan has higher product quality. The method has the advantages of simple process, environmental protection, short production period of products, safe and wide sources of raw materials, reduction of waste of water resources in the extraction process, and avoidance of discharge of waste liquid generated in the extraction process, and is a novel green preparation method.)

1. A preparation method of Kappa carrageenan gum liquid is characterized by comprising the following steps:

placing K type Eucheuma Gelatinosum in Ca (OH)₂In a solution environment;

heating to melt the glue;

introducing CO₂To react with Ca (OH)₂Reaction to form CaCO₃；

Filtering to obtain Kappa carrageenan glue solution.

2. The method of claim 1, wherein the CO is introduced in step₂To react with Ca (OH)₂Reaction to form CaCO₃The method comprises the following steps of filtering to obtain Kappa carrageenan glue solution:

further introducing CO₂With CaCO₃Reaction to form Ca (HCO)₃)₂。

3. The method of claim 2, wherein the CO is introduced in step₂To react with Ca (OH)₂Reaction to form CaCO₃Is and intoIntroducing CO in one step₂With CaCO₃Reaction to form Ca (HCO)₃)₂"further comprising the following steps:

pre-filtering to obtain filtrate.

4. The production method according to any one of claims 1 to 3, characterized in that:

the Ca (OH)₂The solution environment is composed of Ca (OH)₂And water according to the weight-volume ratio of 1g:1000mL to 1g:10 mL.

5. The production method according to any one of claims 1 to 3, characterized in that:

the Ca (OH)₂The solution environment is obtained by mixing CaO and water according to the weight-volume ratio of 0.757g:1000mL to 0.757g:10 mL.

6. The production method according to any one of claims 1 to 3, characterized in that:

the heating temperature range is 80 ℃ to 110 ℃.

7. The production method according to any one of claims 1 to 3, characterized in that:

the length of time of the heating ranges from 4 hours to 16 hours.

8. The production method according to any one of claims 1 to 3, characterized in that:

the K type Eucheuma Gelatinosum with Ca (OH)₂The weight-to-volume ratio of the solution is 1g:15mL to 1g:35 mL.

9. The production method according to any one of claims 1 to 3, characterized in that:

the K-type eucheuma is cleaned and cut up in advance.

10. The production method according to any one of claims 1 to 3, characterized in that:

an appropriate amount of KCl was added to gel the carrageenan before or after filtration, or before or after prefiltration.

11. A process for the preparation of Kappa carrageenan powder comprising the steps of the process according to any one of claims 1 to 10, further comprising the steps of:

coagulating, dehydrating, drying and crushing the obtained Kappa carrageenan glue solution.

Technical Field

The invention relates to the field of carrageenan processing, and in particular relates to a preparation method of Kappa carrageenan glue solution.

Background

Carrageenan is a natural anionic sulfated linear polysaccharide extracted from red algae. Carrageenan has a wide range of applications, not only is used in various food ingredients, but also is a good source of soluble fiber. The carrageenan has good gelling property, easily obtained raw materials and good transparency and clarity of colloid, and is applied to the production of bread, jelly, ice cream and other foods at present.

At present, the extraction process of carrageenan mainly comprises three modes of alkaline extraction, enzymatic extraction and enzymatic auxiliary extraction, wherein the alkaline extraction is usually carried out by using strong alkali such as NaOH and KOH, the alkali treatment time is long, the alkali consumption is large, the polysaccharide chain is seriously depolymerized in the process, the yield and the characteristics of the carrageenan are finally influenced, and the extraction process not only depends on alkaline impregnation, but also requires higher extraction temperature and longer extraction time for mechanical stirring and continuous energy consumption. In addition, the waste alkali liquor generated in the cleaning process in the extraction process needs to be neutralized by acid, and the obtained high-salinity wastewater is difficult to treat and causes great pollution to the surrounding environment, so that the production enterprise has heavy burden in the aspects of energy consumption and environmental protection.

Therefore, in order to solve the problems of large pollution, easy degradation of carrageenan, low extraction yield and the like caused by using a large amount of strong bases such as NaOH or KOH in the existing carrageenan extraction process, it is necessary to establish an environment-friendly extraction production process so as to promote the sustainable development of the carrageenan production and processing industry.

Disclosure of Invention

The invention provides a preparation method of Kappa carrageenan glue solution, which comprises the following steps:

placing Eucheuma gelatinae K in Ca (OH)2 solution;

heating to melt the glue;

introducing CO2 to react with Ca (OH)2 to generate CaCO 3;

filtering to obtain Kappa carrageenan glue solution.

Further, between the steps of introducing CO2 to react with Ca (OH)2 to generate CaCO3 and filtering to obtain Kappa carrageenan gel liquid, the method also comprises the following steps:

further CO2 was passed to react with CaCO3 to form Ca (HCO3) 2.

Further, between the steps of "introducing CO2 to react with Ca (OH)2 to produce CaCO 3" and "further introducing CO2 to react with CaCO3 to produce Ca (HCO3) 2", the method also comprises the following steps:

pre-filtering to obtain filtrate.

Further, the Ca (OH)2 solution environment is obtained by mixing Ca (OH)2 and water according to the weight-volume ratio of 1g:1000mL to 1g:10 mL.

Further, the Ca (OH)2 solution environment is obtained by mixing CaO and water according to the weight-volume ratio of 0.757g:1000mL to 0.757g:10 mL.

Further, the heating temperature ranges from 80 ℃ to 110 ℃.

Further, the length of time of the heating ranges from 4 hours to 16 hours.

Further, the weight-to-volume ratio of the Eucheuma K to the Ca (OH)2 solution is 1g:15mL to 1g:35 mL.

Further, the K-type eucheuma is cleaned and cut up in advance.

Further, an appropriate amount of KCl was added before or after filtration, or before or after prefiltering to gel the carrageenan.

A preparation method of Kappa carrageenan powder comprises the steps of any one of the preparation methods, and further comprises the following steps:

coagulating, dehydrating, drying and crushing the obtained Kappa carrageenan glue solution.

Drawings

FIG. 1 shows Ca (OH) according to an embodiment of the present invention₂The influence of the solution feed liquid ratio on the gel strength of the carrageenan;

FIG. 2 is a graph of the effect of reaction time on carrageenan gel strength according to an embodiment of the present invention;

FIG. 3 is a graph of the effect of process temperature on carrageenan gel strength according to an embodiment of the present invention;

FIG. 4 is a graph of the effect of algae water ratio on carrageenan gel strength according to an embodiment of the invention;

FIG. 5 is a graph of the effect of feedstock pretreatment on carrageenan gel strength according to an embodiment of the present invention;

FIG. 6 is a graph showing the effect of the redissolution of carrageenan powder according to an embodiment of the present invention;

FIG. 7 is a pH test of carrageenan powder after dissolution according to an embodiment of the invention.

Detailed Description

The technical solution of the present invention is illustrated by specific examples below. It is to be understood that one or more method steps mentioned in the present invention do not exclude the presence of other method steps before or after the combination step or that other method steps may be inserted between the explicitly mentioned steps; it should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.

In order to better understand the above technical solutions, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention have been shown, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

The test materials used in the embodiments of the present invention are all commercially available products, and are all commercially available.

Example 1

Weighing 25g of K-type eucheuma respectively, and cleaning for later use. According to the weight-volume ratio of 1:1000, 1:200, 1:100, 1:40, 1:20 and 1:10 (unit: g/mL), respectively, adding Ca (OH)₂Adding into water, stirring, and dissolving completely. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above solutions, stirring, and decocting in 100 deg.C water bath for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Due to CO₂And Ca (OH)₂Reaction to form CaCO₃When the glue solution is turbid, continuously introducing CO₂Stopping introducing CO when the pH value of the glue solution is 8-10₂Weighing 30g of potassium chloride according to the proportion of 1:300 (the weight of the potassium chloride: the volume of the glue solution), dissolving a small amount of water, pouring the water into the glue solution, fully stirring, filtering by using a double-layer cotton 200-mesh filter cloth, cooling and solidifying the obtained filtrate, dehydrating, drying, and crushing to obtain the carrageenan powder.

The carrageenan powder obtained in this example was tested with Ca (OH)₂The gel strength of the carrageenan shows a trend of increasing and then decreasing when the concentration is increased, when the concentration is Ca (OH)₂When the ratio of the treatment liquid to the treatment liquid is 1:200, the gel strength of the carrageenan reaches the maximum value, and the gel strength is (1017.5 +/-23.5) g/cm²As in fig. 1. The yield of carrageenin powder is 31.68 percent.

The gel strength of carrageenan in this example and other examples or comparative examples was calculated as follows:

preparing 1.5% (W/V) Kappa carrageenan solution (containing 0.2% of KCl), heating in boiling water bath until the solution is completely dissolved, pouring the gum solution into a dish with the diameter of 90mm, cooling and solidifying at room temperature, covering with a preservative film, and standing at 20 ℃ for 15 h. Placing the plate to be measured on the left tray of the tray balance, and placing the plate with the sectional area of 1cm²The plunger piston is fixed after just contacting the surface of the gel, a beaker is placed on a tray on the right side of the balance, distilled water is poured uniformly and slowly, pouring of the distilled water is stopped immediately after the surface of the gel is broken, and the weight of the beaker and the distilled water at the moment is recorded, namely the gel strength of the carrageenan.

Gel Strength (g.cm)^-2)＝M/S

In the formula: m-total weight of distilled water, unit: g;

s-plunger cross-sectional area, unit: cm²。

The formula for calculating the yield of carrageenan in this example and other examples or comparative examples is as follows:

the yield of carrageenan (m) (%)_CarrageenanX (1-moisture content). times.100/[ m_{Eucheuma muricatum}X (1-moisture content)]

In the formula: m is_{Eucheuma muricatum}-weight of non-pretreated eucheuma, unit: g;

m_carrageenanThe weight of the dried carrageenan powder is as follows: g.

wherein, the moisture content is measured by reference to GB 5009.3-2016.

Example 2

Respectively weighing 25g of 5 parts of K-type eucheuma, and cleaning for later use. Ca (OH) with a ratio of formulation to liquid of 1:200₂And (4) treating the liquid. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above solutions, stirring, placing in 100 deg.C water bath, and decocting for 4h, 5h, 6h, 7h, and 8 h. Then, CO2 was introduced into the glue solution by using an air distribution tube, since CO2 and Ca (OH)₂Reaction to form CaCO₃When the glue solution is turbid, continuously introducing CO₂Stopping introducing CO when the pH value of the glue solution is 8-10₂Weighing 30g of potassium chloride according to the proportion of 1:300 (the weight of the potassium chloride: the volume of the glue solution), dissolving a small amount of the potassium chloride in water, pouring the water into the glue solution, fully stirring, filtering by using double-layer cotton 200-mesh filter cloth, cooling and solidifying the obtained filtrate, dehydrating, drying, and crushing to obtain the carrageenan powder.

According to the carrageenan powder obtained in the embodiment, the gel strength of the carrageenan is continuously increased along with the extension of the gel boiling time, and the carrageenan is in a trend of approximately increasing linearly and is gradually reduced to 8 hours. After 8h of treatment, the gel strength of the obtained carrageenan is (1336.4 +/-106.5) g/cm²As shown in fig. 2. The yield of carragheenan gum powder is 29.92%.

Example 3

Respectively weighing 25g of 5 parts of K-type eucheuma, and cleaning for later use. Ca (OH) with a ratio of formulation to liquid of 1:200₂And (4) treating the liquid. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above solutions, stirring, and decocting in water bath at 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, and 100 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Due to CO₂And Ca (OH)₂Reaction to form CaCO₃When the glue solution is turbid, continuously introducing CO₂Stopping introducing CO when the pH value of the glue solution is 8-10₂Weighing 30g of potassium chloride according to the proportion of 1:300 (the weight of the potassium chloride: the volume of the glue solution), dissolving a small amount of water, pouring the glue solution into the glue solution, fully stirring, filtering by using a double-layer cotton-sandwiched 200-mesh filter cloth, cooling and solidifying the obtained filtrate, dehydrating, drying, and crushing to obtain the carrageenan powder.

According to the carrageenan powder obtained in the embodiment, the gel strength of the carrageenan shows a gradually rising trend along with the rising of the gel boiling temperature through detection, and the carrageenan powder is boiledWhen the temperature reaches 100 ℃, the gel strength increases and flattens, and is (1075.0 +/-17.5) g/cm²As shown in figure 3, the yield of carrageenan powder is 28.40%.

Example 4

Respectively weighing 25g of 5 parts of K-type eucheuma, and cleaning for later use. Ca (OH) with a ratio of formulation to liquid of 1:200₂The treatment solutions were mixed at a ratio of 1:15, 1:20, 1:25, 1:30, 1:35 (W), respectively_{Eucheuma muricatum}:V_{Feed liquid}) The ratio of algae to water of Eucheuma Gelatinosum and Ca (OH)₂Mixing the treating solutions, and boiling in 100 deg.C water bath for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Due to CO₂And Ca (OH)₂Reaction to form CaCO₃When the glue solution is turbid, continuously introducing CO₂Stopping introducing CO when the pH value of the glue solution is 8-10₂Weighing 30g of potassium chloride according to the proportion of 1:300 (the weight of the potassium chloride: the volume of the glue solution), dissolving a small amount of water, fully stirring, filtering by using double-layer cotton-sandwiched 200-mesh filter cloth, cooling and solidifying the obtained filtrate, dehydrating, drying, and crushing to obtain the carrageenan powder.

The carrageenin powder obtained in the embodiment is detected to have a slow growth trend of the algae-water ratio between 1:15 and 1:30, and the change is not obvious on the whole. The gel strength decreased significantly at 1:35, as shown in FIG. 4. As can be seen, the algae-laden water ratio has an influence on the gel strength of carrageenan in the present example, and the gel strength is the highest (1281.1 + -72.2) g/cm when the algae-laden water ratio is 1:30²The yield of carragheen powder is 27.40%.

Example 5

Weighing 25g of K-type eucheuma in 5 parts respectively, pretreating in five modes of uncut section, crushing and sieving with a 40-mesh sieve, crushing and sieving with a 60-mesh sieve and crushing and sieving with a 80-mesh sieve respectively, and cleaning for later use. Ca (OH) with a ratio of formulation to liquid of 1:200₂The treatment solution was then mixed at 1:30 (W)_{Eucheuma muricatum}:V_{Feed liquid}) The ratio of algae to water of Eucheuma Gelatinosum and Ca (OH)₂Mixing the above solutions, stirring, and decocting in 100 deg.C water bath for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Due to CO₂And Ca (OH))₂Reaction to form CaCO₃When the glue solution is turbid, continuously introducing CO₂Stopping introducing CO when the pH value of the glue solution is 8-10₂Weighing 30g of potassium chloride according to the proportion of 1:300 (the weight of the potassium chloride: the volume of the glue solution), dissolving a small amount of water, fully stirring, filtering by using double-layer cotton-sandwiched 200-mesh filter cloth, cooling and solidifying the obtained filtrate, dehydrating, drying, and crushing to obtain the carrageenan powder.

According to the carrageenan powder obtained in the embodiment, through detection, the carrageenan powder is subjected to crushing, 80-mesh sieve treatment and then is boiled, and the gel strength of the obtained carrageenan is the highest and is (1508.1 +/-20.6) g/cm²As shown in fig. 5. The yield of carrageenin powder is 31.08%.

Example 6

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:200₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above processed solutions, stirring, and decocting at 100 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Stopping introducing CO when the pH value is about 8₂Adding 1Kg of KCl (firstly, pre-dissolving with a little water), fully stirring, filtering with a plate frame, subpackaging the obtained filtrate in a stainless steel disc, cooling, solidifying, bagging, dehydrating under pressure, drying, and pulverizing to obtain carrageenan powder.

The carrageenin powder obtained in the embodiment is detected to have the pH of 9.24, the moisture content of 11.46%, the gel strength of 1276g/cm2, the viscosity of 145mPa & s, the transparency of 43.2%, the whiteness of 71.2% and the ash content of 26.33%.

The viscosity, transparency, whiteness and ash content in the examples and other examples and comparative examples were measured by methods known to those skilled in the art

Example 7

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:100₂Added to water and stirred to dissolve it thoroughly. Then, the process of the present invention is carried out,in a ratio of 1:30 (W)_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above processed solutions, stirring, and decocting at 100 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Stopping introducing CO when the pH value is about 8₂Adding 1Kg of KCl (firstly, pre-dissolving with a little water), fully stirring, filtering with a plate frame, subpackaging the obtained filtrate in a stainless steel disc, cooling, solidifying, bagging, dehydrating under pressure, drying, and pulverizing to obtain carrageenan powder.

The carrageenin powder obtained in the embodiment has the advantages of pH 9.56, moisture content 9.31% and gel strength 1102g/cm through detection²Viscosity 58 mPas, transparency 53.8%, whiteness 76.9% and ash content 22.55%.

Example 8

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:100₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the solutions, stirring, and decocting at 100 deg.C for 12 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Stopping introducing CO when the pH value is about 8₂Adding 1Kg of KCl (firstly, pre-dissolving with a little water), fully stirring, filtering with a plate frame, subpackaging the obtained filtrate in a stainless steel disc, cooling, solidifying, bagging, dehydrating under pressure, drying, and pulverizing to obtain carrageenan powder.

The carrageenin powder obtained in the embodiment has the advantages of pH 10.09, water content 10.34% and gel strength 1789g/cm through detection²Viscosity 115 mPas, transparency 80.6%, whiteness 76.9% and ash content 20.35%.

Example 9

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:200₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) "will be kylinVegetables and Ca (OH)₂Mixing the above processed solutions, stirring, and decocting under pressure at 110 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Continuously introducing CO₂Until the glue solution is clear, then stopping introducing CO₂Adding 1Kg of KCl (firstly, pre-dissolving with a little water), fully stirring, filtering with a plate frame, subpackaging the obtained filtrate in a stainless steel disc, cooling, solidifying, bagging, dehydrating under pressure, drying, and pulverizing to obtain carrageenan powder.

The carrageenin powder obtained in the embodiment has the advantages of pH 7.25, water content of 12.26% and gel strength of 1770g/cm through detection²Viscosity 104 mPas, transparency 94.1%, whiteness 80.4%, ash 19.65%.

Example 10

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:200₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above processed solutions, stirring, and decocting at 100 deg.C for 16 hr. Then, an air distribution pipe is adopted, CO2 is introduced into the glue solution, the glue solution is stirred, the turbidity gradually appears, CaCO is generated₃Stopping introducing CO when the pH value is about 8₂Adding 1Kg of KCl (firstly, pre-dissolving with a little water), fully stirring, filtering with a plate frame, subpackaging the obtained filtrate in a stainless steel disc, cooling, solidifying, bagging, dehydrating under pressure, drying, and pulverizing to obtain carrageenan powder.

The carrageenin powder obtained in the embodiment has the pH of 9.98, the moisture content of 12.62 percent and the gel strength of 1704g/cm through detection²Viscosity 90 mPas, transparency 69.8%, whiteness 80.1%, ash 20.25%.

Example 11

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:100₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above processed solutions, stirring, and decocting at 100 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Stopping introducing CO when the pH value is about 8₂Adding 1Kg of KCl (firstly, pre-dissolving with a little water), fully stirring uniformly, and filtering by adopting a plate frame; introducing CO into the obtained filtrate again₂Stopping introducing CO when the filtrate is completely clear₂And subpackaging the obtained filtrate in a stainless steel disc, cooling and solidifying, bagging, dehydrating under pressure, drying, and crushing to obtain the carrageenan powder.

The carrageenin powder obtained in the embodiment has the pH of 8.56, the water content of 9.91 percent and the gel strength of 1232g/cm through detection²Viscosity 67 mPas, transparency 55.8%, whiteness 78.6%, ash 20.55%.

Example 12

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:200₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Eucheuma Gelatinosum and Ca (OH)₂Mixing the above processed solutions, stirring, and decocting under pressure at 110 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Continuously introducing CO₂Until the glue solution is clear, then stopping introducing CO₂Filtering; adding industrial ethanol into the filtrate at a ratio of 1:1(V: V) for alcohol precipitation, drying the obtained gelatin block, and pulverizing to obtain carrageenan powder.

The carrageenin powder obtained in the embodiment has the pH of 7.95, the moisture content of 11.76 percent and the gel strength of 1700g/cm through detection²Viscosity 123 mPas, transparency 95.8%, whiteness 82.4% and ash content 18.25%.

Example 13

Weighing 10Kg of K type eucheuma, and cleaning for later use. Mixing Ca (OH) according to the proportion of 1:200₂Added to water and stirred to dissolve it thoroughly. Then, in a ratio (W) of 1:30_{Eucheuma muricatum}:V_{Feed liquid}) Mixing Eucheuma Gelatinosum and Ca (OH))₂Mixing the above processed solutions, stirring, and decocting at 100 deg.C for 8 hr. Then, an air distribution pipe is adopted to introduce CO into the glue solution₂Stirring to make the glue solution become turbid gradually and generate CaCO₃Stopping introducing CO when the pH value is about 8₂Filtering; introducing CO into the obtained filtrate again₂Stopping introducing CO when the filtrate is completely clear₂(ii) a Then adding industrial ethanol according to the proportion of 1:1(V: V) for alcohol precipitation, drying and crushing the obtained rubber block, and finally obtaining the carrageenan powder.

The carrageenin powder obtained in the embodiment has the advantages of pH 8.74, moisture content of 10.96% and gel strength of 1366g/cm²Viscosity 115 mPas, transparency 65.2%, whiteness 76.2% and ash content 22.33%.

The following table is a summary of the results of the Kappa carrageenan performance tests made in examples 6-13:

examples 8, 9, 10 supplementary experiments:

the carrageenan powder obtained by the extraction in the examples 8, 9 and 10 was redissolved, and the obtained gum solution was as shown in FIG. 6. It can be seen that the carrageenan powders obtained in examples 8 and 10 were cloudy after dissolution, indicating that the powders had passed through CO₂After neutralization, Ca (OH)₂Formation of CaCO₃Resulting in turbidity of the glue. Cooling and solidifying the glue solution, dehydrating, drying and crushing to obtain carrageenin powder, wherein CaCO in the carrageenin powder₃Not removed completely, and re-dissolved to a liquid gel which appeared cloudy.

The clarity of the carrageenan powder obtained in example 9 was found to be 94.1% after dissolution, indicating that Ca (OH)₂By CO₂Neutralization to form CaCO₃Continuously introducing CO₂，CaCO₃Formation of Ca (HCO)₃)₂，Ca(HCO₃)₂Dissolved in water and becomes transparent. And cooling and solidifying the glue solution, dehydrating, drying and crushing to obtain the carrageenan powder.

To determine the carats obtained in examples 8, 9 and 10Ca (HCO) in rubber powder₃)₂If the current signal exists, test verification is carried out, and the result is shown in the attached figure 7.

The carrageenin sample No. 1 adopts the traditional sodium hydroxide extraction process, and the carrageenin solution is clear; carrageenan powder from example 9 above, No. 2, dissolved in water, essentially as in No. 1, the solution appeared clear; the glue powder used in No. 3 is the same as that used in No. 2, but the pH value of the glue solution is adjusted to about 10, and the clarity of the glue solution is still very high, which indicates that most of Ca (HCO)₃)₂Has been separated out with water, and the calcium salt content in the rubber powder is very little.

Comparative example 1-Kappa carrageenan extracted by conventional Process

Weighing 25g of K type eucheuma, and cleaning for later use. Preparing a mixed treatment solution of NaOH and KCl, wherein the concentration of NaOH is 10 percent (W)_NaOH:V_{Water (W)}) The concentration of KCl is 12% (W)_KCl:V_{Water (W)}). Then, the eucheuma is added into the mixed treatment liquid according to the proportion of 1:30, after the mixed treatment liquid is treated for 4 hours at 65 ℃, a large amount of tap water is used for repeatedly rinsing until the material liquid is neutral, and then water is added for soaking overnight. Adding water at a ratio of 1:20, decocting to obtain a liquid gel, filtering, cooling the filtrate to about 55 deg.C, and mixing at 1:1 (V)_{KCl solution}:V_Filtrate) Adding a KCl solution of 5% (W/V, the same below) for salting out, dehydrating the obtained rubber block, drying and crushing to obtain the Kappa carrageenan powder.

The Kappa carrageenan powder extracted by the process is detected to have the gel strength of 1627g/cm²The yield of carragheenan gum powder is 23.5%.

Comparative example 2

Weighing 25g of K type eucheuma, and cleaning for later use. Adding tap water into Eucheuma at a ratio of 1:30, and boiling in a 100 deg.C water bath for 8 hr. Filtering the obtained glue solution with double-layer cotton-sandwiched 200-mesh filter cloth while it is hot, and mixing the obtained filtrate with 1:1 (V)_Filtrate：V_{KCl solution}) Mixing the salt with a 5% KCl solution, and salting out; the obtained rubber block is dehydrated, dried and crushed to obtain the carrageenan powder.

The carrageenin powder obtained by the comparative example has the gel strength after detectionIs (382.5 +/-13.9) g/cm²The yield of carragheen powder is 34.80%. Thus, it can be seen that, in the carrageenan extraction process, if Ca (OH) is not added₂The obtained carrageenan has very low gel strength and is Ca (OH)₂The carrageenan gel strength of the boiled gelatin is greatly improved.

Comparative example 3

Weighing 25g of K type eucheuma, and cleaning for later use. Adding water into Eucheuma Gelatinosum according to the feed liquid ratio of 1:30, and boiling the mixture in a water bath kettle at 100 ℃ for 8 h. Filtering the obtained glue solution with double-layer cotton-sandwiched 200-mesh filter cloth while it is hot, and mixing the obtained filtrate with 1:1 (V)_Filtrate： V_{KCl solution}) Mixing the salt with a 5% KCl solution, and salting out; the obtained rubber block is dehydrated, dried and crushed to obtain the carrageenan powder. Taking 1.5g of carrageenan powder and 0.2g of KCl, adding 100mL of water into a 500mL beaker to prepare 1.5% (W/V) carrageenan solution, adding 2g of anhydrous calcium chloride, uniformly stirring, heating for dissolving, finally pouring into a culture dish of 90mm, and detecting the gel strength.

The carrageenin powder obtained by the comparative example has the gel strength (188.4 +/-13.6) g/cm through detection²The yield of carragheen powder was 21.35%. It can be seen from this that, the Ca (OH)₂Improvement of gel strength of carrageenin powder extracted after treatment and Ca²⁺Not related to the alkaline action of calcium hydroxide.

In conclusion, compared with the comparative example, the carrageenan powder prepared by the embodiment of the invention has the advantages that the gel strength is obviously improved, and the yield is relatively improved. Thereby passing Ca (OH)₂The solution is combined with the boiling process of the gelatin, and then CO is used₂Removal of Ca (OH)₂The solution can prepare the carrageenan with high gel strength and high yield, so that the carrageenan has higher product quality. The method has the advantages of simple process, environmental protection, short production period of products, safe and wide sources of raw materials, reduction of waste of water resources in the extraction process, and avoidance of discharge of waste liquid generated in the extraction process, and is a novel green extraction process.

In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above should not be understood to necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.

Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.