CN114586892A - Preparation method of rapidly-dispersed tannate protein granules - Google Patents

Preparation method of rapidly-dispersed tannate protein granules Download PDF

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Publication number
CN114586892A
CN114586892A CN202210178059.4A CN202210178059A CN114586892A CN 114586892 A CN114586892 A CN 114586892A CN 202210178059 A CN202210178059 A CN 202210178059A CN 114586892 A CN114586892 A CN 114586892A
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parts
mass ratio
preparing
sodium
diatomite
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王珊
郭华
刘宇
王良
李春阳
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Jiayijia Biotech Inc
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Jiayijia Biotech Inc
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A23K20/10—Organic substances
    • A23K20/142—Amino acids; Derivatives thereof
    • A23K20/147—Polymeric derivatives, e.g. peptides or proteins
    • A—HUMAN NECESSITIES
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Abstract

A preparation method of a fast-dispersing tannate protein granule comprises the steps of preparing a filler, preparing a dispersing agent, preparing a disintegrating agent and preparing the granule. The tannate protein granules prepared by the invention have good dispersibility, high suspension rate in water, suspension rate of 98.7-98.8% and no sediment at the bottom; the tannate protein granules prepared by the invention have high heat storage stability, are dispersed in water and are placed for 14 days at 54 ℃, the suspension rate is 98.5-98.6%, and no precipitate exists at the bottom; the tannate protein granules prepared by the invention have good disintegration performance, and can be completely disintegrated within 12-13 s.

Description

Preparation method of rapidly-dispersed tannate protein granules
Technical Field
The invention relates to a preparation method of rapidly-dispersed tannate protein granules, and belongs to the technical field of feed additives.
Background
The tannase can be used for treating diarrhea, is a medicine shared by human and livestock, and is not listed in banning resistance list because the tannase is of plant source. For human administration, tablets and "water-soluble" tablets are generally used, the water-soluble being "emulsions" obtained by mixing the tannase with a surfactant and then adding to water. Most of the tannate protein for livestock is added into feed, and is prepared into different dosage forms to be applied to the feed by ingestion and taking, which is the basis for finally solving the problem of livestock feeding. For young livestock with diarrhea, the young livestock is weak in constitution and difficult to eat, the more effective administration mode is water aqua drenching, the dosage is more accurately mastered, the administration mode of people can be introduced into livestock feeding, and the tannase is prepared into particles and water dispersible granules which can be rapidly dispersed in water, so that the treatment of the diarrhea of the livestock is convenient.
CN107281110A discloses a tannic acid protein powder capable of being administered by drinking water and a preparation method thereof, wherein the index of the dispersibility is only the uniform dispersion without sedimentation, only the qualitative index of the dispersibility of the powder is described, and the index of the suspension rate representing the dispersibility is not disclosed, and the tannic acid protein powder can cause sedimentation after being dispersed in water for a long time, becomes an inhomogeneous suspension state, and does not disclose the disintegration performance.
CN1689639 discloses a tannate protein quick disintegrating preparation and its preparation method, which can shorten its disintegration time, can be completely disintegrated within one minute, the disintegration time is still slow, and its dispersing property after disintegration is poor, and it can not form uniform suspension.
CN110870478A discloses a solid preparation containing biphenyl compounds and application thereof, which improves the suspension performance of the solid preparation, the optimal scheme can reach 98% suspension rate at normal temperature, and the suspension rate can still be maintained at 98% at 14 days at 54 ℃, but the disintegration speed is slow, and the solid preparation cannot be rapidly dispersed in water.
The existing granular product prepared from the tannic protein often has the defects of slow disintegration, poor suspension rate after disintegration and dispersion and incapability of forming uniform suspension.
In summary, the prior art has the following problems:
(1) the existing tannate protein granules have poor dispersion performance and low suspension rate, the suspension rate is reduced along with the increase of time, and the heat storage stability is poor;
(2) the existing tannalbin granules are slow in disintegration.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art, and the invention realizes the following aims by preparing a fast-dispersing tannate protein granule by improving a filler, a dispersing agent and a disintegrating agent and adding other components:
(1) the tannase protein granules have good dispersibility, high suspension rate, good thermal storage stability and no reduction of the suspension rate along with the increase of time;
(2) the tannalbin granule has high disintegration speed.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a fast-dispersing tannate protein granule is characterized by comprising the steps of preparing a filler, preparing a dispersing agent, preparing a disintegrating agent and preparing the granule.
The following is a further improvement of the above technical solution:
the filler preparation comprises the steps of preparing modified diatomite and mixing;
the modified diatomite is prepared by mixing diatomite with deionized water, adding p-toluenesulfonic acid, soaking for 180-250min at 25-35 ℃, then adding hydrogen peroxide, heating to 65-75 ℃ and keeping for 50-70min, cooling, then adding gamma-glycidyl ether oxypropyltrimethoxysilane and n-butyl alcohol, carrying out microwave treatment for 10-30min under the power of 90-120W, heating to 90-100 ℃, stirring for 350-400min, filtering, washing and drying to obtain the modified diatomite;
mixing, namely stirring a mixture of modified diatomite, corn starch, white carbon black, polyoxyethylene fatty alcohol ether and water at 45-55 ℃ for 25-40min, drying at 70-85 ℃ to constant weight, and crushing to obtain a filler;
the mass ratio of the diatomite to the deionized water is 1: 4-6;
the mass ratio of the p-toluenesulfonic acid to the diatomite is 1.5-2.5: 1;
the mass ratio of the hydrogen peroxide to the toluenesulfonic acid is 2-4: 10;
the mass concentration of the hydrogen peroxide is 25-35%;
the mass ratio of the gamma-glycidyl ether oxypropyl trimethoxysilane to the diatomite is 1: 14-16;
the mass ratio of the n-butanol to the diatomite is 1: 4-6;
the mixture comprises the following components in parts by mass: 60-80 parts of modified diatomite, 15-25 parts of corn starch, 8-12 parts of white carbon black, 4-6 parts of polyoxyethylene fatty alcohol ether and 80-120 parts of water.
Mixing sodium lignosulfonate with deionized water, adding concentrated hydrochloric acid and sodium chlorate, stirring at 35-45 ℃ for 14-16h, adding absolute ethyl alcohol to precipitate modified sodium lignosulfonate, filtering, washing with absolute ethyl alcohol, and drying to obtain modified sodium lignosulfonate;
the mass ratio of the sodium lignin sulfonate to the deionized water is 1: 9-11;
the mass ratio of the concentrated hydrochloric acid to the sodium lignin sulfonate is 1: 2.5-3.5;
the mass ratio of the sodium chlorate to the sodium lignosulfonate is 1: 1.8-2.2;
the mass ratio of the absolute ethyl alcohol to the sodium lignin sulfonate is 7-9: 1.
The preparation of the disintegrating agent comprises the steps of mixing and dissolving sodium carboxymethyl starch with deionized water, adding glycidyl trimethyl ammonium chloride and sodium chloride, stirring at 60-70 ℃ for 200-260min, filtering, cleaning and drying to obtain modified sodium carboxymethyl starch, uniformly mixing the modified sodium carboxymethyl starch with palm oil and ammonium sulfate, putting the mixture into a high-pressure homogenizer to perform three times of homogenization circulation at 700-900bar, and performing spray drying to obtain the disintegrating agent;
the mass ratio of the sodium carboxymethyl starch to the deionized water is 1: 14-16;
the mass ratio of the glycidyl trimethyl ammonium chloride to the sodium carboxymethyl starch is 1.5-2.5: 5;
the mass ratio of the sodium chloride to the sodium carboxymethyl starch is 1: 18-22;
the mass ratio of the palm oil to the modified sodium carboxymethyl starch is 0.8-1.2: 2;
the mass ratio of the ammonium sulfate to the modified sodium carboxymethyl starch is 1: 2.5-3.5.
The preparation method comprises the steps of uniformly mixing the tannage protein and the modified sodium lignosulfonate, adding the filler, the disintegrant, the camellia seed powder, the caprylyl capric ester, the soap powder and the emulsified silicone oil, uniformly mixing while spraying pure water and stirring, simultaneously spraying the rapeseed oil, uniformly mixing, adding the maltodextrin and the lactose, pressing into granules, and drying to obtain the rapidly-dispersed tannage protein granules;
the tannalbin granule comprises the following raw materials in parts by mass: 25-35 parts of tannase protein, 8-12 parts of modified sodium lignosulfonate, 40-60 parts of filler, 8-12 parts of disintegrating agent, 4-6 parts of camellia seed powder, 1.8-2.2 parts of caprylic capric ester, 1.8-2.2 parts of soap powder, 1.8-2.2 parts of emulsified silicone oil, 40-60 parts of pure water, 4-6 parts of rapeseed oil, 2.5-3.5 parts of maltodextrin and 1.8-2.2 parts of lactose.
Compared with the prior art, the invention has the following beneficial effects:
the tannate protein granules prepared by the invention have good dispersibility, high suspension rate when the granules are dispersed in water, the suspension rate is 98.7-98.8%, and no precipitate is generated at the bottom (GB/T14825-2006);
the tannalbin granules prepared by the invention have high heat storage stability, are dispersed in water and are placed for 14 days at 54 ℃, the suspension rate is 98.5-98.6%, and no precipitate exists at the bottom (GB/T19136-;
the tannate protein granules prepared by the invention have good disintegration performance, and can be completely disintegrated within 12-13 s;
the tannalbin granules prepared by the invention have little foaming after dispersion, and the foam volume is 5.4-5.6ml (GB/T28137-;
the tannate protein granules prepared by the invention have good wetting performance and short wetting time which is 17-19s (GB/T5451-2001).
Detailed Description
Example 1
(1) Preparation of the Filler
a. Preparation of modified diatomaceous Earth
Mixing diatomite with deionized water, adding p-toluenesulfonic acid, soaking at 30 ℃ for 200min, then adding hydrogen peroxide, heating to 70 ℃ and keeping for 60min, cooling, then adding gamma-glycidoxypropyltrimethoxysilane and n-butanol, carrying out microwave treatment for 15min under the power of 100W, heating to 100 ℃, stirring for 360min, filtering, washing and drying to obtain modified diatomite;
the mass ratio of the diatomite to the deionized water is 1: 5;
the mass ratio of the p-toluenesulfonic acid to the diatomite is 2: 1;
the mass ratio of the hydrogen peroxide to the toluenesulfonic acid is 3: 10;
the mass concentration of the hydrogen peroxide is 30 percent;
the mass ratio of the gamma-glycidyl ether oxypropyl trimethoxysilane to the diatomite is 1: 15;
the mass ratio of the n-butanol to the diatomite is 1: 5;
b. mixing
Stirring a mixture of modified diatomite, corn starch, white carbon black, polyoxyethylene fatty alcohol ether and water at 50 ℃ for 30min, drying at 80 ℃ to constant weight, and crushing to obtain a filler;
the mixture comprises the following components in parts by mass: 70 parts of modified diatomite, 20 parts of corn starch, 10 parts of white carbon black, 5 parts of polyoxyethylene fatty alcohol ether and 100 parts of water.
(2) Preparation of the dispersant
Mixing sodium lignosulfonate with deionized water, adding concentrated hydrochloric acid and sodium chlorate, stirring at 40 ℃ for 15 hours, adding absolute ethyl alcohol to precipitate modified sodium lignosulfonate, filtering, washing with absolute ethyl alcohol, and drying to obtain modified sodium lignosulfonate;
the mass ratio of the sodium lignin sulfonate to the deionized water is 1: 10;
the mass ratio of the concentrated hydrochloric acid to the sodium lignin sulfonate is 1: 3;
the mass ratio of the sodium chlorate to the sodium lignosulfonate is 1: 2;
the mass ratio of the absolute ethyl alcohol to the sodium lignin sulfonate is 8: 1.
(3) Preparation of disintegrating agent
Mixing sodium carboxymethyl starch with deionized water to completely dissolve the sodium carboxymethyl starch, adding glycidyl trimethyl ammonium chloride and sodium chloride, stirring at 65 ℃ for 240min, filtering, cleaning and drying to obtain modified sodium carboxymethyl starch, uniformly mixing the modified sodium carboxymethyl starch with a certain amount of palm oil and ammonium sulfate, putting the mixture into a high-pressure homogenizer to perform three times of homogenization circulation at 800bar, and performing spray drying to obtain a disintegrant;
the mass ratio of the sodium carboxymethyl starch to the deionized water is 1: 15;
the mass ratio of the glycidyl trimethyl ammonium chloride to the sodium carboxymethyl starch is 2: 5;
the mass ratio of the sodium chloride to the sodium carboxymethyl starch is 1: 20;
the mass ratio of the palm oil to the modified sodium carboxymethyl starch is 1: 2;
the mass ratio of the ammonium sulfate to the modified sodium carboxymethyl starch is 1:3.
(4) Preparing into granule
Adding the tannalbin and the modified sodium lignosulfonate into an enamel plate, uniformly mixing, adding the filler, the disintegrant, the camellia seed powder, the caprylic sunflower ester, the soap powder and the emulsified silicone oil, uniformly mixing, spraying pure water while stirring, spraying the rapeseed oil, uniformly mixing, adding a certain amount of maltodextrin and lactose, pressing into granules, putting into the enamel plate, and drying at 60 ℃ to obtain the rapidly-dispersed tannalbin granules;
the tannalbin granule comprises the following raw materials in parts by mass: 30 parts of tannase protein, 10 parts of modified sodium lignosulfonate, 50 parts of filler, 10 parts of disintegrating agent, 5 parts of camellia seed powder, 2 parts of caprylic sunflower ester, 2 parts of soap powder, 2 parts of emulsified silicone oil, 50 parts of pure water, 5 parts of rapeseed oil, 3 parts of maltodextrin and 2 parts of lactose.
The tannate protein granules prepared in the embodiment 1 have good dispersibility, high suspension rate in water, 98.8% of suspension rate and no sediment at the bottom (GB/T14825-2006);
the tannase protein granules prepared in example 1 have high heat storage stability, are dispersed in water and are placed for 14 days at 54 ℃, the suspension rate is 98.6 percent, and no precipitate exists at the bottom (GB/T19136-;
the tannate protein granules prepared in example 1 have good disintegration performance, and can be completely disintegrated within 12 s;
the tannase protein granules prepared in example 1 have little foaming after dispersion, and the foam volume is 5.4ml (GB/T28137-;
the tannic acid protein granules prepared in the example 1 have good wetting property and short wetting time which is 17s (GB/T5451-2001).
Example 2
(1) Preparation of the Filler
a. Preparation of modified diatomaceous Earth
Mixing diatomite with deionized water, adding p-toluenesulfonic acid, soaking at 25 ℃ for 180min, then adding hydrogen peroxide, heating to 65 ℃ and keeping for 70min, cooling, then adding gamma-glycidoxypropyltrimethoxysilane and n-butanol, carrying out microwave treatment for 30min under the power of 90W, heating to 90 ℃, stirring for 400min, filtering, washing and drying to obtain modified diatomite;
the mass ratio of the diatomite to the deionized water is 1: 4;
the mass ratio of the p-toluenesulfonic acid to the diatomite is 1.5: 1;
the mass ratio of the hydrogen peroxide to the toluenesulfonic acid is 2: 10;
the mass concentration of the hydrogen peroxide is 35 percent;
the mass ratio of the gamma-glycidyl ether oxypropyl trimethoxysilane to the diatomite is 1: 14;
the mass ratio of the n-butanol to the diatomite is 1: 4;
b. mixing
Stirring a mixture of modified diatomite, corn starch, white carbon black, polyoxyethylene fatty alcohol ether and water at 45 ℃ for 40min, drying at 70 ℃ to constant weight, and crushing to obtain a filler;
the mixture comprises the following components in parts by mass: 60 parts of modified diatomite, 15 parts of corn starch, 8 parts of white carbon black, 4 parts of polyoxyethylene fatty alcohol ether and 80 parts of water.
(2) Preparation of the dispersant
Mixing sodium lignosulfonate with deionized water, adding concentrated hydrochloric acid and sodium chlorate, stirring at 35 ℃ for 14h, adding absolute ethyl alcohol to precipitate modified sodium lignosulfonate, filtering, washing with absolute ethyl alcohol, and drying to obtain modified sodium lignosulfonate;
the mass ratio of the sodium lignosulfonate to the deionized water is 1: 9;
the mass ratio of the concentrated hydrochloric acid to the sodium lignin sulfonate is 1: 2.5;
the mass ratio of the sodium chlorate to the sodium lignosulfonate is 1: 1.8;
the mass ratio of the absolute ethyl alcohol to the sodium lignin sulfonate is 7: 1.
(3) Preparation of disintegrating agent
Mixing sodium carboxymethyl starch with deionized water to completely dissolve the sodium carboxymethyl starch, adding glycidyl trimethyl ammonium chloride and sodium chloride, stirring at 60 ℃ for 260min, filtering, cleaning and drying to obtain modified sodium carboxymethyl starch, uniformly mixing the modified sodium carboxymethyl starch with a certain amount of palm oil and ammonium sulfate, putting the mixture into a high-pressure homogenizer to perform three times of homogenization circulation at 700bar, and performing spray drying to obtain a disintegrant;
the mass ratio of the sodium carboxymethyl starch to the deionized water is 1: 14;
the mass ratio of the glycidyl trimethyl ammonium chloride to the sodium carboxymethyl starch is 1.5: 5;
the mass ratio of the sodium chloride to the sodium carboxymethyl starch is 1: 18;
the mass ratio of the palm oil to the modified sodium carboxymethyl starch is 0.8: 2;
the mass ratio of the ammonium sulfate to the modified sodium carboxymethyl starch is 1: 2.5.
(4) Preparing into granule
Adding the tannic protein and the modified sodium lignosulfonate into an enamel plate, uniformly mixing, adding the filler, the disintegrant, the camellia seed powder, the caprylic sunflower ester, the soap powder and the emulsified silicone oil, uniformly mixing, spraying pure water while stirring, spraying the rapeseed oil, uniformly mixing, adding a certain amount of maltodextrin and lactose, pressing into granules, putting into the enamel plate, and drying at 55 ℃ to obtain a rapidly-dispersed tannic protein granule;
the tannalbin granule comprises the following raw materials in parts by mass: 25 parts of tannase protein, 8 parts of modified sodium lignosulfonate, 40 parts of filler, 8 parts of disintegrating agent, 4 parts of camellia seed powder, 1.8 parts of caprylic capric ester, 1.8 parts of soap powder, 1.8 parts of emulsified silicone oil, 40 parts of pure water, 4 parts of rapeseed oil, 2.5 parts of maltodextrin and 1.8 parts of lactose.
The tannate protein granules prepared in the embodiment 2 have good dispersibility, high suspension rate in water, 98.7% of suspension rate and no sediment at the bottom (GB/T14825-;
the tannase protein granules prepared in example 2 have high heat storage stability, are dispersed in water and are placed for 14 days at 54 ℃, the suspension rate is 98.6 percent, and no precipitate exists at the bottom (GB/T19136-;
the tannate protein granules prepared in example 2 have good disintegration performance, and can be completely disintegrated within 13 s;
the tannase protein granules prepared in example 2 have little foaming after dispersion, and the foam volume is 5.6ml (GB/T28137-;
the tannate protein granules prepared in example 2 have good wetting property and short wetting time, and the wetting time is 18s (GB/T5451-2001).
Example 3
(1) Preparation of the Filler
a. Preparation of modified diatomaceous Earth
Mixing diatomite with deionized water, adding p-toluenesulfonic acid, soaking at 35 ℃ for 250min, then adding hydrogen peroxide, heating to 75 ℃ and keeping for 50min, cooling, then adding gamma-glycidyl ether oxypropyltrimethoxysilane and n-butanol, performing microwave treatment at 120W power for 10min, then heating to 100 ℃, stirring for 350min, filtering, washing and drying to obtain modified diatomite;
the mass ratio of the diatomite to the deionized water is 1: 6;
the mass ratio of the p-toluenesulfonic acid to the diatomite is 2.5: 1;
the mass ratio of the hydrogen peroxide to the toluenesulfonic acid is 4: 10;
the mass concentration of the hydrogen peroxide is 25 percent;
the mass ratio of the gamma-glycidyl ether oxypropyl trimethoxysilane to the diatomite is 1: 16;
the mass ratio of the n-butanol to the diatomite is 1: 6;
b. mixing
Stirring a mixture of modified diatomite, corn starch, white carbon black, polyoxyethylene fatty alcohol ether and water at 550 ℃ for 25min, drying at 85 ℃ to constant weight, and crushing to obtain a filler;
the mixture comprises the following components in parts by mass: 80 parts of modified diatomite, 25 parts of corn starch, 12 parts of white carbon black, 6 parts of polyoxyethylene fatty alcohol ether and 120 parts of water.
(2) Preparation of the dispersant
Mixing sodium lignosulfonate with deionized water, adding concentrated hydrochloric acid and sodium chlorate, stirring at 45 ℃ for 16 hours, adding absolute ethyl alcohol to precipitate modified sodium lignosulfonate, filtering, washing with absolute ethyl alcohol, and drying to obtain modified sodium lignosulfonate;
the mass ratio of the sodium lignosulfonate to the deionized water is 1: 11;
the mass ratio of the concentrated hydrochloric acid to the sodium lignin sulfonate is 1: 3.5;
the mass ratio of the sodium chlorate to the sodium lignosulfonate is 1: 2.2;
the mass ratio of the absolute ethyl alcohol to the sodium lignin sulfonate is 9: 1.
(3) Preparation of disintegrating agent
Mixing sodium carboxymethyl starch with deionized water to completely dissolve the sodium carboxymethyl starch, adding glycidyl trimethyl ammonium chloride and sodium chloride, stirring at 70 ℃ for 200min, filtering, cleaning and drying to obtain modified sodium carboxymethyl starch, uniformly mixing the modified sodium carboxymethyl starch with a certain amount of palm oil and ammonium sulfate, putting the mixture into a high-pressure homogenizer to perform three times of homogenization circulation at 900bar, and performing spray drying to obtain a disintegrant;
the mass ratio of the sodium carboxymethyl starch to the deionized water is 1: 16;
the mass ratio of the glycidyl trimethyl ammonium chloride to the sodium carboxymethyl starch is 2.5: 5;
the mass ratio of the sodium chloride to the sodium carboxymethyl starch is 1: 22;
the mass ratio of the palm oil to the modified sodium carboxymethyl starch is 1.2: 2;
the mass ratio of the ammonium sulfate to the modified sodium carboxymethyl starch is 1: 3.5.
(4) Preparing into granule
Adding the tannic protein and the modified sodium lignosulfonate into an enamel plate, uniformly mixing, adding the filler, the disintegrant, the camellia seed powder, the caprylic sunflower ester, the soap powder and the emulsified silicone oil, uniformly mixing, spraying pure water while stirring, spraying the rapeseed oil, uniformly mixing, adding a certain amount of maltodextrin and lactose, pressing into granules, putting into the enamel plate, and drying at 65 ℃ to obtain a rapidly-dispersed tannic protein granule;
the tannalbin granule comprises the following raw materials in parts by mass: 35 parts of tannase protein, 12 parts of modified sodium lignosulfonate, 60 parts of filler, 12 parts of disintegrating agent, 6 parts of camellia seed powder, 2.2 parts of caprylic sunflower ester, 2.2 parts of soap powder, 2.2 parts of emulsified silicone oil, 60 parts of pure water, 6 parts of rapeseed oil, 3.5 parts of maltodextrin and 2.2 parts of lactose.
The tannate protein granules prepared in the embodiment 3 have good dispersibility, high suspension rate in water, the suspension rate is 98.7%, and no sediment is left at the bottom (GB/T14825-2006);
the tannase protein granules prepared in example 3 have high heat storage stability, are dispersed in water and are placed for 14 days at 54 ℃, the suspension rate is 98.5 percent, and no precipitate exists at the bottom (GB/T19136-;
the tannate protein granules prepared in example 3 have good disintegration performance, and can be completely disintegrated within 13 s;
the tannalbin granules prepared in example 3 have little foaming after dispersion, and the foam volume is 5.5ml (GB/T28137-;
the tannic acid protein granules prepared in the example 3 have good wetting property and short wetting time which is 19s (GB/T5451-2001).
Comparative example 1
On the basis of example 1, the step of preparing the filler is omitted, modified diatomite is prepared, the unmodified diatomite is used for preparing the filler, in the mixing step, a mixture of the unmodified diatomite, corn starch, white carbon black, polyoxyethylene fatty alcohol ether and water is stirred for 30min at 50 ℃, dried to constant weight at 80 ℃, crushed to obtain the filler, and the rest steps are the same, so that granules are prepared;
the mixture comprises the following components in parts by mass: 70 parts of unmodified diatomite, 20 parts of corn starch, 10 parts of white carbon black, 5 parts of polyoxyethylene fatty alcohol ether and 100 parts of water.
The suspension rate of the tannalbin granules prepared in the comparative example 1 is 94.1%, and a little precipitate exists at the bottom (GB/T14825-2006);
the tannalbin granules prepared in comparative example 1 were left at 54 ℃ for 14 days, the suspension rate was 91.7%, and a little precipitate was formed at the bottom (GB/T19136-;
the tannalbin granules 17s prepared in comparative example 1 were completely disintegrated;
the tannase protein granules prepared in comparative example 1 have a foam volume of 6.3ml (GB/T28137-;
the tannase granules prepared in comparative example 1 had a wetting time of 23s (GB/T5451-2001).
Comparative example 2
On the basis of the example 1, the step of preparing a dispersing agent is omitted, unmodified sodium lignosulfonate is used as the dispersing agent in the step of preparing the granules, and the rest steps are the same to prepare the granules;
the granules comprise the following raw materials in parts by mass: 30 parts of tannase protein, 10 parts of sodium lignosulfonate, 50 parts of filler, 10 parts of disintegrating agent, 5 parts of camellia seed powder, 2 parts of caprylic sunflower ester, 2 parts of soap powder, 2 parts of emulsified silicone oil, 50 parts of pure water, 5 parts of rapeseed oil, 3 parts of maltodextrin and 2 parts of lactose.
The suspension rate of the tannalbin particle prepared in comparative example 2 is 91.6%, and a little precipitate exists at the bottom (GB/T14825-2006);
the tannalbin granules prepared in comparative example 2 were left at 54 ℃ for 14 days, with a suspension rate of 87.2% and a precipitate at the bottom (GB/T19136-;
the tannalbin granules prepared in comparative example 2 were completely disintegrated in 18 s;
the tannase protein granules prepared in comparative example 2 have a foam volume of 7.1ml (GB/T28137-;
the tannase granules prepared in comparative example 2 had a wetting time of 21s (GB/T5451-2001).
Comparative example 3
On the basis of example 1, a step of preparing a disintegrant was omitted, and a granule was prepared using only ammonium sulfate and sodium carboxymethyl starch as a mixed disintegrant, with the same steps as the rest;
the mass ratio of the ammonium sulfate to the sodium carboxymethyl starch in the mixed disintegrating agent is 1: 3;
the granules comprise the following raw materials in parts by mass: 30 parts of tannase protein, 10 parts of modified sodium lignosulfonate, 50 parts of filler, 10 parts of mixed disintegrating agent, 5 parts of camellia seed powder, 2 parts of caprylic sunflower ester, 2 parts of soap powder, 2 parts of emulsified silicone oil, 50 parts of pure water, 5 parts of rapeseed oil, 3 parts of maltodextrin and 2 parts of lactose.
The suspension rate of the tannalbin granules prepared in the comparative example 3 is 96.5%, and no obvious precipitate is generated at the bottom (GB/T14825-2006);
the albumin tannate granules prepared in comparative example 3 were left at 54 ℃ for 14 days, the suspension rate was 94.2%, and a little precipitate was formed at the bottom (GB/T19136-Astro 2003);
the tannalbin granules 34s prepared in comparative example 3 were completely disintegrated;
the tannase protein granules prepared in comparative example 3 have a foam volume of 6.5ml (GB/T28137-;
the tannalbin granules prepared in comparative example 3 had a wetting time of 24s (GB/T5451-2001).

Claims (10)

1. A preparation method of a fast-dispersing tannate protein granule is characterized by comprising the steps of preparing a filler, preparing a dispersing agent, preparing a disintegrating agent and preparing the granule.
2. The method for preparing the rapidly dispersible tannase protein granules according to claim 1, wherein the method comprises the following steps:
the filler preparation comprises the steps of preparing modified diatomite and mixing;
the modified diatomite is prepared by mixing diatomite with deionized water, adding p-toluenesulfonic acid, soaking for 180-fold organic silicon for 250min, adding hydrogen peroxide, heating to 65-75 ℃ and keeping for 50-70min, cooling, adding gamma-glycidyl ether oxypropyl trimethoxysilane and n-butyl alcohol, performing microwave treatment for 10-30min under the power of 90-120W, heating to 90-100 ℃ and stirring for 350-fold organic silicon for 400min, filtering, washing and drying to obtain the modified diatomite.
3. The method for preparing rapidly dispersing tannase protein granules according to claim 2, wherein:
the mass ratio of the diatomite to the deionized water is 1: 4-6;
the mass ratio of the p-toluenesulfonic acid to the diatomite is 1.5-2.5: 1;
the mass ratio of the hydrogen peroxide to the toluenesulfonic acid is 2-4: 10;
the mass concentration of the hydrogen peroxide is 25-35%;
the mass ratio of the gamma-glycidyl ether oxypropyl trimethoxysilane to the diatomite is 1: 14-16;
the mass ratio of the n-butanol to the diatomite is 1: 4-6.
4. The method for preparing the rapidly dispersible tannase protein granules according to claim 2, wherein the method comprises the following steps:
and mixing, namely stirring the mixture of the modified diatomite, the corn starch, the white carbon black, the polyoxyethylene fatty alcohol ether and the water for 25-40min, drying to constant weight and crushing to obtain the filler.
5. The method for preparing the rapidly dispersible tannase protein granules according to claim 4, wherein the method comprises the following steps:
the mixture comprises the following components in parts by mass: 60-80 parts of modified diatomite, 15-25 parts of corn starch, 8-12 parts of white carbon black, 4-6 parts of polyoxyethylene fatty alcohol ether and 80-120 parts of water.
6. The method for preparing the rapidly dispersible tannase protein granules according to claim 1, wherein the method comprises the following steps:
the preparation method comprises the steps of mixing sodium lignosulfonate with deionized water, adding concentrated hydrochloric acid and sodium chlorate, stirring for 14-16 hours, adding absolute ethyl alcohol to precipitate modified sodium lignosulfonate, filtering, washing with absolute ethyl alcohol, and drying to obtain modified sodium lignosulfonate.
7. The method for preparing the rapidly dispersible tannase protein granules according to claim 6, wherein the method comprises the following steps:
the mass ratio of the sodium lignin sulfonate to the deionized water is 1: 9-11;
the mass ratio of the concentrated hydrochloric acid to the sodium lignin sulfonate is 1: 2.5-3.5;
the mass ratio of the sodium chlorate to the sodium lignin sulfonate is 1: 1.8-2.2;
the mass ratio of the absolute ethyl alcohol to the sodium lignin sulfonate is 7-9: 1.
8. The method for preparing the rapidly dispersible tannase protein granules according to claim 1, wherein the method comprises the following steps:
the preparation method of the disintegrating agent comprises the steps of mixing and dissolving sodium carboxymethyl starch with deionized water, adding glycidyl trimethyl ammonium chloride and sodium chloride, stirring at 60-70 ℃ for 260min, filtering, cleaning and drying to obtain modified sodium carboxymethyl starch, uniformly mixing the modified sodium carboxymethyl starch with palm oil and ammonium sulfate, putting the mixture into a high-pressure homogenizer to perform three times of homogenization circulation at 700-900bar, and performing spray drying to obtain the disintegrating agent.
9. The method for preparing the rapidly dispersible tannase protein granules according to claim 8, wherein the method comprises the following steps:
the mass ratio of the sodium carboxymethyl starch to the deionized water is 1: 14-16;
the mass ratio of the glycidyl trimethyl ammonium chloride to the sodium carboxymethyl starch is 1.5-2.5: 5;
the mass ratio of the sodium chloride to the sodium carboxymethyl starch is 1: 18-22;
the mass ratio of the palm oil to the modified sodium carboxymethyl starch is 0.8-1.2: 2;
the mass ratio of the ammonium sulfate to the modified sodium carboxymethyl starch is 1: 2.5-3.5.
10. The method for preparing the rapidly dispersible tannase protein granules according to claim 1, wherein the method comprises the following steps:
uniformly mixing the tannic protein and the modified sodium lignosulfonate, adding the filler, the disintegrant, the camellia seed powder, the caprylic sunflower ester, the soap powder and the emulsified silicone oil, uniformly mixing while spraying pure water, uniformly mixing while spraying the rapeseed oil, adding the maltodextrin and the lactose, pressing into granules, and drying to obtain the rapidly-dispersed tannic protein granules;
the granules comprise the following raw materials in parts by mass: 25-35 parts of tannase protein, 8-12 parts of modified sodium lignosulfonate, 40-60 parts of filler, 8-12 parts of disintegrating agent, 4-6 parts of camellia seed powder, 1.8-2.2 parts of caprylic capric ester, 1.8-2.2 parts of soap powder, 1.8-2.2 parts of emulsified silicone oil, 40-60 parts of pure water, 4-6 parts of rapeseed oil, 2.5-3.5 parts of maltodextrin and 1.8-2.2 parts of lactose.
CN202210178059.4A 2022-02-25 2022-02-25 Preparation method of rapidly-dispersed tannate protein granules Pending CN114586892A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1689639A (en) * 2004-04-27 2005-11-02 合肥霄云科技有限公司 Tannalbin rapid disintegration preparation and preparing method thereof
CN102450257A (en) * 2011-11-25 2012-05-16 安阳市全丰农药化工有限责任公司 Choline chloride effervescent granule/effervescent tablet and preparation method thereof
CN103348975A (en) * 2012-08-22 2013-10-16 安阳市全丰农药化工有限责任公司 Choline chloride water dispersible granule/tablet and preparation method thereof
CN107281110A (en) * 2017-07-20 2017-10-24 山东福美乐动物药业有限公司 A kind of tannalbin soluble powder and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1689639A (en) * 2004-04-27 2005-11-02 合肥霄云科技有限公司 Tannalbin rapid disintegration preparation and preparing method thereof
CN102450257A (en) * 2011-11-25 2012-05-16 安阳市全丰农药化工有限责任公司 Choline chloride effervescent granule/effervescent tablet and preparation method thereof
CN103348975A (en) * 2012-08-22 2013-10-16 安阳市全丰农药化工有限责任公司 Choline chloride water dispersible granule/tablet and preparation method thereof
CN107281110A (en) * 2017-07-20 2017-10-24 山东福美乐动物药业有限公司 A kind of tannalbin soluble powder and preparation method

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