CN107641159B - A kind of production process of low viscosity whitening carrageenan - Google Patents

Abstract

The invention discloses a production process of low-viscosity whitening carrageenan. The method includes the following steps: washing and removing impurities, adding a compound solution with a concentration of 9-12 wt% sodium hydroxide and 10-13 wt% potassium chloride; Pour off the lye, rinse until neutral; add water to soak at a certain ratio of material to liquid, then add disodium EDTA, adjust the pH value to 3.5~4.5 with acid, then add an appropriate amount of H ₂ O ₂ solution, treat 0.5~ 2 h, filter, rinse to neutrality; add an appropriate amount of sodium hypochlorite solution for treatment for 2~4 h, filter, rinse to neutrality; drain water, dry, dry and pulverize to obtain crude carrageenan. In the present invention, H ₂ O ₂ is used in the extraction process to process the raw material unicornis so as to obtain the carrageenan crude gum with low viscosity, low strength and improved whiteness.

Description

A kind of production process of low viscosity whitening carrageenan

technical field

The invention relates to the technical field of extracting carrageenan from kylin cabbage, in particular to a production process of low-viscosity whitening carrageenan.

Background technique

Carrageenan, also known as carrageenan and carrageenan, is a kind of water-soluble polysaccharide extracted from red algae such as carrageenan. A straight-chain polysaccharide sulfate formed by the combination of D-galactopyranosyl. Carrageenan has the properties of gelation, thickening, emulsification, film formation, stable dispersion, etc. It is widely used in food industries such as candy, meat, dairy products, and brewing. Carrageenan can also be used as a carrier for microbial and immobilized cell research. In addition, carrageenan is also used in the pharmaceutical industry such as sustained-release capsules/tablets, ointment bases, and cod liver oil emulsifiers.

The traditional extraction process of carrageenan is to use NaOH-KCl to process and extract the carrageenan. However, the carrageenan obtained by this method has high viscosity and is not easy to dissolve, which greatly limits the application of carrageenan. Liu Xueping used KOH to alkali-treat Kirin cabbage to obtain carrageenan with lower viscosity and better quality. Li Guicun used H ₂ O ₂ to degrade k-carrageenan to obtain a lower molecular weight carrageenan and improve the solubility of carrageenan. However, there is no report on using H ₂ O ₂ to process Kirin cabbage in the extraction process to obtain low-viscosity carrageenan. In view of this, the inventors have researched and designed a production process of low-viscosity whitening carrageenan, and this case is born.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a kind of production process of low viscosity whitening carrageenan, adopt cleaning chemical reagent H ₂ O ₂ to carry out processing on the extraction process of unicornis, thereby obtain the carrageenan with low viscosity, low strength, whiteness improvement Compared with the chemical modification of the finished carrageenan, the production cost is reduced, and H ₂ O ₂ is a clean and non-polluting chemical reagent, which can be reused and is suitable for industrial production.

In order to achieve the above object, the technical scheme adopted by the present invention is as follows:

A production process of low-viscosity whitening carrageenan, comprising the following steps:

Step 1, raw material cleaning: take an appropriate amount of dried kylin cabbage, add 20 to 100 times by weight of clean water to rinse, remove impurities;

Step 2. Alkali treatment: add lye to the washed kylin cabbage, the ratio of material to liquid is 1:20 ~ 1:100g/ml, soak at a constant temperature of 55 ~ 70 ℃ for 3 ~ 6 hours, filter out the lye, and use clean water Soak and rinse until neutral;

Step 3, low viscosity treatment: add water according to a certain ratio of material to liquid, then add a metal chelating agent with a final concentration of 0.012wt% disodium EDTA, adjust the pH value with hydrochloric acid to 3-5, and add a final concentration of 0.25-1.5 wt % H ₂ O ₂ , treated at room temperature for 0.5 to 2 h, stirred intermittently during the period, filtered, and the filter residue was rinsed to neutrality;

Step 4, bleaching treatment: add water to the filter residue obtained in step 3 according to the ratio of material to liquid 1:30 g/ml, then add an appropriate amount of bleaching water, treat for 2 to 4 h, filter, and rinse to neutrality;

Step 5. Finished product: Drain the water of the bleached kylin cabbage, dry it in the air, pulverize and sieve, and collect the powder.

As the preferred mode of embodiment, in above-mentioned step 1, the material-water ratio of cleaning kylin cabbage is 1:30～1:50 g/ml;

As the preferred mode of the embodiment, in the above-mentioned steps 2, the lye is the compound solution of 9～12wt% sodium hydroxide and 10～13wt% potassium chloride, preferably 10wt% sodium hydroxide and 12wt% potassium chloride The compound solution was treated at a constant temperature of 63 °C for 4 h;

As the preferred mode of the embodiment, in the above-mentioned steps 3, the material-to-liquid ratio is 1:30 g/ml, and the final concentration of disodium EDTA is 0.012wt%;

As the preferred mode of the embodiment, in the above-mentioned step 3, the pH value of the low-viscosity treatment is 3.8~4.2;

As the preferred mode of the embodiment, in the above-mentioned step 3, the final concentration of the used H ₂ O ₂ solution in the low-viscosity treatment system is 0.25-1.5 wt %, and the treatment is carried out at room temperature for 1-2 h;

As the preferred mode of embodiment, in above-mentioned steps 4, the consumption of bleaching water is one twentieth of the weight of kylin cabbage, and the treatment time is 2～3 h;

As the preferred mode of the embodiment, in the above-mentioned step 5, after draining the water, the unicorn cabbage is dried in the sun, and further dried in a 55 ℃ oven, and after being pulverized, it is passed through an 80-mesh sieve for use.

After the above scheme is adopted in the present invention, under acidic conditions, the carrageenan molecule is degraded by H ₂ O ₂ treatment on the kylin, thereby reducing the viscosity of the carrageenan.

Detailed ways

Example 1

Raw material cleaning: take 30 g of dried kylin cabbage, add 1000 ml of water to rinse, remove impurities;

Alkali treatment: Add the compound lye solution of sodium hydroxide and potassium chloride with concentrations of 10wt% and 12wt% respectively, the ratio of material to liquid is 1:30g/ml, soak at a constant temperature of 63 ℃ for 4 h, and filter out the lye solution , soak and rinse several times with water;

Bleaching treatment: add water to the alkali-treated Kirin cabbage at a ratio of 1:30 g/ml of material to liquid, adjust the pH to about 7 with hydrochloric acid, then add 1.5 ml of bleaching water, treat for 3 hours, filter, and rinse until neutral;

Finished product: After draining the water of the kylin cabbage, place it in a tray to dry in the sun, and further dry it at 55 °C, then pulverize it, pass it through an 80-mesh sieve, and collect the powder.

The bleaching water used is a sodium hypochlorite stock solution with an effective chlorine content of 8%.

The carrageenan coarse rubber powder obtained in this example has a viscosity of 130.0 mPa·s, a gel strength of 560 g/cm ² and a whiteness of 29.9 % after testing.

Example 2

Raw material cleaning: take 30 g of dried kylin cabbage, add 1000 ml of water to rinse, remove impurities;

Alkaline treatment: add 800 ml of a compound lye solution of sodium hydroxide and potassium chloride with concentrations of 10 wt% and 12 wt% respectively, soak at a constant temperature of 63 °C for 4 h, filter out the lye solution, soak in water and rinse to medium sex;

Low-viscosity treatment: Add water to the alkali-treated Kirin cabbage at a material-to-liquid ratio of 1:30 g/ml, then add a metal chelating agent with a final concentration of 0.012 wt% disodium EDTA, adjust the pH to 4.0 with hydrochloric acid, add The final concentration was 0.5 wt% H ₂ O ₂ , treated at room temperature for 1 h, stirred intermittently during the period, filtered, and the filter residue was rinsed to neutrality;

Bleaching treatment: add water to the filter residue after low viscosity treatment according to the ratio of material to liquid 1:30g/ml, then add 1.5 ml bleaching water, treat for 3 hours, filter, and rinse until neutral;

Finished product: After draining the water of the kylin cabbage, place it in a tray to dry in the sun, and further dry it at 55 °C, then pulverize it, pass it through an 80-mesh sieve, and collect the powder.

The bleaching water used is a sodium hypochlorite stock solution with an effective chlorine content of 8%.

The carrageenan coarse rubber powder obtained in this example has a viscosity of 112.2 mPa·s, a gel strength of 433 g/cm ² and a whiteness of 35.2 % after testing.

Example 3

Raw material cleaning: take 30 g of dried kylin cabbage, add 1000 ml of water to rinse, remove impurities;

Alkali treatment: add 800 ml of a compound lye solution of sodium hydroxide and potassium chloride with concentrations of 10 wt% and 12 wt% respectively, soak at a constant temperature of 63 °C for 4 h, filter out the lye solution, soak and rinse with water until neutral ;

Low-viscosity treatment: Add water to the alkali-treated Kirin cabbage at a ratio of material to liquid of 1:30 g/ml, then add disodium EDTA metal chelating agent with a final concentration of 0.012 wt%, adjust the pH value to 4.0 with hydrochloric acid, and add a final concentration of 0.012 wt%. The concentration is 1.0 wt% H ₂ O ₂ , treated at room temperature for 1 h, stirred intermittently during the period, filtered, and the filter residue was rinsed to neutrality;

Bleaching treatment: add water to the filter residue after low viscosity treatment according to the ratio of material to liquid 1:30g/ml, then add 1.5 ml bleaching water, treat for 3 hours, filter, and rinse until neutral;

Finished product: After draining the water of the kylin cabbage, place it in a tray to dry in the sun, and further dry it at 55 °C, then pulverize it, pass it through an 80-mesh sieve, and collect the powder.

The bleaching water used is a sodium hypochlorite stock solution with an effective chlorine content of 8%.

The carrageenan coarse rubber powder obtained in this example has a viscosity of 101.5 mPa·s, a gel strength of 430 g/cm ² and a whiteness of 40.1 % after testing.

Example 4

Raw material cleaning: take 30 g of dried kylin cabbage, add 1000 ml of water to rinse, remove impurities;

Alkaline treatment: add 800 ml of a compound lye solution of sodium hydroxide and potassium chloride with concentrations of 10 wt% and 12 wt% respectively, soak at a constant temperature of 63 °C for 4 h, filter out the lye solution, soak in water and rinse to medium sex;

Low-viscosity treatment: Add water to the alkali-treated Kirin cabbage at a ratio of material to liquid of 1:30 g/ml, then add disodium EDTA metal chelating agent with a final concentration of 0.012 wt%, adjust the pH value to 4.0 with hydrochloric acid, and add a final concentration of 0.012 wt%. The concentration is 1.5 wt% H ₂ O ₂ , treated at room temperature for 1 h, stirred intermittently during the period, filtered, and the filter residue was rinsed to neutrality;

Bleaching treatment: add water to the filter residue after low viscosity treatment according to the ratio of material to liquid 1:30g/ml, then add 1.5 ml bleaching water, treat for 3 hours, filter, and rinse until neutral;

Finished product: After draining the water of the kylin cabbage, place it in a tray to dry in the sun, and further dry it at 55 °C, then pulverize it, pass it through an 80-mesh sieve, and collect the powder.

The bleaching water used is a sodium hypochlorite stock solution with an effective chlorine content of 8%.

The carrageenan coarse rubber powder obtained in this example has a viscosity of 85.0 mPa·s, a gel strength of 459 g/cm ² and a whiteness of 37.6 % after testing.

Example 5

Raw material cleaning: take 60 g of dried kylin cabbage, add 2000 ml of water to rinse, remove impurities;

Alkali treatment: add 1600ml of compound lye solution of sodium hydroxide and potassium chloride with concentrations of 10wt% and 12wt% respectively, soak at a constant temperature of 63 ℃ for 4 h, filter out the lye solution, soak and rinse with water until neutral;

Low-viscosity treatment: Add water to the alkali-treated Kirin cabbage at a ratio of material to liquid of 1:30 g/ml, then add disodium EDTA metal chelating agent with a final concentration of 0.012 wt%, adjust the pH value to 4.0 with hydrochloric acid, and add a final concentration of 0.012 wt%. The concentration is 1.5 wt% H ₂ O ₂ , treated at room temperature for 1 h, stirred intermittently during the period, filtered, and the filter residue was rinsed to neutrality;

Bleaching treatment: add water to the filter residue after low viscosity treatment at a ratio of 1:30g/ml of material to liquid, then add 3.0 ml of bleaching water, treat for 3 hours, filter, and rinse until neutral;

Finished product: After draining the water of the kylin cabbage, place it in a tray to dry in the sun, and further dry it at 55 °C, then pulverize it, pass it through an 80-mesh sieve, and collect the powder.

The bleaching water used is a sodium hypochlorite stock solution with an effective chlorine content of 8%.

The carrageenan coarse rubber powder obtained in this example has a viscosity of 86.2 mPa·s, a gel strength of 460 g/cm ² and a whiteness of 38.9 % after testing.

The present invention adopts H ₂ O ₂ in the extraction process of carrageenan to process kylin, so as to realize chemical modification of carrageenan, obtain products with new properties, and open up the application field of carrageenan. The H ₂ O ₂ used is a clean and non-polluting chemical reagent, which can be reused and is suitable for the industrial production of enterprises.

The main property parameters are shown in Table 1:

Table 1 Comparison table of main property parameters of the carrageenan coarse rubber powder obtained in Examples 1-5

As can be seen from the data in Table 1, the process of the present invention has a certain viscosity-reducing effect on carrageenan, and at the same time, also has different degrees of influence on the gel strength and whiteness of carrageenan, wherein the gel strength is reduced, and the whiteness is slightly. improve. This is because H ₂ O ₂ has a strong oxidizing effect, which leads to a decrease in the molecular weight of carrageenan, so the viscosity and gel strength of carrageenan decrease. The bleaching effect of H ₂ O ₂ makes the whiteness of carrageenan treated with H ₂ O ₂ improved to a certain extent.

The above embodiments are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. All modifications that those of ordinary skill in the art can directly derive or associate from the disclosure of the present invention should be considered as the protection scope of the present invention.

Claims (6)

1. a production technique of low-viscosity whitening carrageenan, is characterized in that, comprises the steps: Step 1, raw material cleaning: take an appropriate amount of dried kylin cabbage, add 20 to 100 times by weight of clean water to rinse, remove impurities; Step 2. Alkali treatment: add lye to the washed kylin cabbage, the material-to-liquid ratio is 1:20 ~ 1:100, soak at a constant temperature of 55 ~ 70 ° C for 3 ~ 6 h, filter out the lye, soak in clean water, Rinse until neutral; Step 3, low-viscosity treatment: add water to the unicorn after the alkali treatment in step 2 according to the ratio of material to liquid 1:30, then add a final concentration of 0.012wt% EDTA disodium metal chelating agent, adjust the pH value with hydrochloric acid to 3 ~ 5, adding H ₂ O ₂ with a final concentration of 0.25 ~ 1.5wt%, treating at room temperature for 0.5 ~ 2 h, stirring intermittently during the period, filtering, and rinsing the filter residue to neutrality; Step 4. Bleaching treatment: add water to the filter residue obtained in step 3 according to a material-to-liquid ratio of 1:30, then add an appropriate amount of bleaching water, process for 2 to 4 h, filter, and rinse to neutrality; Step 5, finished product: drain the water of the bleached kylin cabbage, dry it in the air, pulverize and sieve, and collect the powder; In step 2, the lye solution is a compound solution of sodium hydroxide and potassium chloride, containing 10 wt% sodium hydroxide and 12 wt% potassium chloride respectively. 2. the production technique of a kind of low viscosity whitening carrageenan according to claim 1, is characterized in that: in step 2, the solid-liquid ratio of alkali treatment is 1:25～1:30, and treatment temperature is 63 ℃, The processing time was 4 h. 3. The production process of a low-viscosity whitening carrageenan according to claim 1, characterized in that: in step 3, the pH value of the low-viscosity treatment is 3.8 to 4.2. 4. The production process of a low-viscosity whitening carrageenan according to claim 1, wherein in step 3, the low-viscosity treatment time is 1-2 h. 5. the production technique of a kind of low-viscosity whitening carrageenan according to claim 1, is characterized in that: in step 4, the bleaching water that adopts is the sodium hypochlorite stoste of 8～10% that the available chlorine content, consumption and Kirin The weight ratio of vegetables was 1:20, and the processing time was 2 to 3 h. 6. The production process of low-viscosity whitening carrageenan according to claim 1, characterized in that: in step 5, kylin cabbage is preferably dried in the sun.