CN108740345B - Sodium humate product containing oligosaccharide and application thereof - Google Patents
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Abstract
A sodium humate product containing oligosaccharide and its application are disclosed, which comprises the following components: 25-30 parts of corncobs, 55-60 parts of humic acid and 10-15 parts of sodium hydroxide. The preparation method comprises the following steps: (1) adding 25-30 parts of corncobs and 5-10 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 150-; (2) adding 55-60 parts of humic acid mineral powder crushed to 60-100 meshes into a reaction kettle; introducing steam, controlling the temperature at 105-120 ℃, stirring and reacting for 1-2 hours to obtain xylo-oligosaccharide, glucose oligosaccharide and a small amount of sodium humate, standing and cooling; (3) adding 5-10 parts of sodium hydroxide into the reaction kettle in the step (2), controlling the temperature to be 70-90 ℃, stirring and reacting for 2-4 hours to obtain oligosaccharide and sodium humate, standing and cooling; (4) centrifuging the reaction solution for 0.5 hour to obtain a centrifugate; (5) placing the centrifugate in a drying sedimentation tank, standing for 6-10 hours, and taking supernatant; (6) drying the supernatant in a roller to obtain flaky particles; the product containing oligosaccharide sodium humate is obtained and used as feed additive for livestock and poultry breeding.
Description
The application is a divisional application of Chinese patent application with the application date of 2015, 10 and 19 and the application number of 2015106747361, which is named as a sodium humate product containing oligosaccharide and preparation and application thereof.
Technical Field
The invention relates to preparation of a sodium humate product containing oligosaccharide and application of the sodium humate product containing oligosaccharide in livestock and poultry breeding, in particular to a method for degrading lignin in corncobs and promoting release of hemicellulose and cellulose by taking corncobs, humic acid and sodium hydroxide as raw materials and reacting the sodium hydroxide with the corncobs; humic acid reacts with hemicellulose and cellulose to generate oligosaccharide; sodium hydroxide reacts with humic acid to generate sodium humate, and sodium humate solution is subjected to centrifugation, precipitation and drying to obtain oligosaccharide-containing sodium humate products.
Background
The negative impact of antibiotic use has been largely documented and it has become imperative to find new antibiotic-free additives that reduce the dependence on antibiotics.
Corncobs consist of lignin, cellulose and hemicellulose, wherein lignin can be degraded by alkali and release cellulose and hemicellulose. Cellulose and hemicellulose can be degraded into oligosaccharides such as glucose oligosaccharide, xylose oligosaccharide, arabinose oligosaccharide and the like under acidic conditions, the oligosaccharides are compounds polymerized by 2-10 glycosidic bonds, can improve the intestinal micro-ecological environment, are beneficial to the proliferation of bifidobacterium and other beneficial bacteria, generate organic acid through metabolism to reduce the pH value in the intestine, inhibit the growth of salmonella and putrefying bacteria in the intestine, regulate the gastrointestinal function, inhibit putrefying substances in the intestine, change the stool property, increase the synthesis of vitamins and improve the immune function of the organism.
Humic acid is a kind of natural organic weak acid, and is a heterogeneous complex mixture in physical chemistry. The mixture is composed of natural, high molecular weight, yellow to black, amorphous, colloidal, fatty and aromatic organic electrolytes, and cannot be represented by a single chemical structural formula. The sodium humate is black brown flaky solid with metallic luster obtained by high-temperature reaction of humic acid and sodium hydroxide, residue separation, concentration and drying.
Sodium humate can adsorb intestinal endotoxin, reduce its to advocating mucosa damage, promote the growth of intestines fine hair, and then improve animal digestion and absorption ability. Meanwhile, as the humic acid has larger molecular weight and can be associated into larger particles in a certain medium, the humic acid has colloid property and adsorption capacity, forms good ion exchange and catalysis effects, promotes the activation and absorption of feed ingredients, further promotes the growth of animals and reduces the feed conversion ratio.
Patent 201210401506.4 discloses a method for obtaining uniform xylan from corn cob by leaching with hot water and sodium hydroxide to obtain high-purity xylan, but a large amount of incompletely decomposed cellulose and hemicellulose are wasted as waste in the reaction process, and the conversion rate and utilization rate of the substrate are reduced. 201310515953.7 discloses a rare earth and sodium humate compound feed additive and its preparation method, the method dries sodium humate by airing, the water insoluble matter content of the product is high and the dried sodium humate needs to be crushed, the time consumption is long, the site demand is increased, the method is influenced by weather, and the method is not beneficial to industrial production. Patent 201310494632.3 discloses a humic acid production technology, in which hydrogen peroxide is used to oxidize humic acid into micromolecular humic acid, and the process can destroy the network molecular structure of humic acid, reduce the capability of humic acid to absorb intestinal toxins in intestinal tracts, and reduce the efficacy of humic acid as a feed additive.
Disclosure of Invention
The invention selects the corncob with low price as the raw material of the oligosaccharide, combines with the production process of the sodium humate, and uses the humic acid and the sodium hydroxide in the production process of the sodium humate to provide the organic acid, the alkali and the reaction device in the production process of the oligosaccharide, thereby reducing the production cost of the oligosaccharide. The oligosaccharide-containing sodium humate produced by the invention simultaneously contains oligosaccharide beneficial to the health of the intestinal tract and sodium humate capable of promoting the development of the intestinal tract, on one hand, the oligosaccharide can promote the growth of beneficial bacteria in the intestinal tract, improve the microecology of the intestinal tract, reduce the proliferation of harmful bacteria in the intestinal tract, reduce the damage of the harmful bacteria to the intestinal tract and promote the health of the intestinal tract; on the other hand, sodium humate adsorbs enteron harmful bacteria such as escherichia coli, salmonella and other secreted toxins, so that damage to intestinal mucosa is reduced, intestinal villus development is promoted, the ratio of intestinal villus to crypt of the intestinal tract is improved, and finally the absorption capacity of the animal intestinal tract to nutrient substances is improved.
The invention also aims to provide the sodium humate preparation containing oligosaccharide, which has important application in the field of livestock and poultry breeding.
The purpose of the invention is realized by the following steps: a sodium humate product containing oligosaccharide is characterized by comprising the following components in parts by weight: 25-30 parts of corncobs, 55-60 parts of humic acid and 10-15 parts of sodium hydroxide.
The invention is also characterized in that the sodium humate product containing oligosaccharide comprises the following components in parts by weight: 28 parts of corncobs, 58 parts of humic acid and 15 parts of sodium hydroxide.
The preparation method of the oligosaccharide-containing sodium humate product is characterized by comprising the following steps:
(1) adding 25-30 parts of corncobs and 5-10 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 150-; (2) adding 55-60 parts of humic acid mineral powder crushed to 60-100 meshes into a reaction kettle; introducing steam, controlling the temperature at 105-120 ℃, stirring and reacting for 1-2 hours to obtain xylo-oligosaccharide, glucose oligosaccharide and a small amount of sodium humate, standing and cooling; (3) adding 5-10 parts of sodium hydroxide into the reaction kettle in the step (2), controlling the temperature to be 70-90 ℃, stirring and reacting for 2-4 hours to obtain oligosaccharide and sodium humate, standing and cooling; (4) centrifuging the reaction solution for 0.5 hour to obtain a centrifugate; (5) placing the centrifugate in a drying sedimentation tank, standing for 6-10 hours, and taking supernatant; (6) drying the supernatant in a roller to obtain flaky particles; thus obtaining the product containing oligosaccharide sodium humate.
The invention is also characterized in that the sodium humate dried by the roller is black. And (4) sieving the flaky particles with a 16-20-mesh sieve to obtain the product containing oligosaccharide sodium humate.
The application of the product containing oligosaccharide sodium humate as feed additive for raising livestock and poultry is disclosed.
The invention is characterized in that the sodium humate product containing oligosaccharide is mixed with feed in a proportion of 0.3 percent and is directly fed to livestock and poultry.
The invention has the beneficial effects that: 1. the production process of the oligosaccharide takes cheap corncobs as raw materials, and necessary humic acid, sodium hydroxide and reaction devices are produced by sodium humate in the production process, so that the equipment investment for producing xylo-oligosaccharide is saved, and the production cost of the oligosaccharide is reduced. 2. The production process of the xylo-oligosaccharide takes humic acid as organic acid for hydrolyzing cellulose and hemicellulose, avoids adding inorganic acid in the production process of the inorganic acid, and simultaneously has no production waste liquid generated compared with the traditional xylo-oligosaccharide production process as part of the production process integrated in the production process of sodium humate, thereby reducing the treatment cost of the waste liquid and avoiding environmental pollution. 3. Sodium hydroxide degrades lignin in the corncobs in a steam environment, so that cellulose and hemicellulose in the corncobs are fully released; humic acid degrades cellulose and hemicellulose into oligosaccharide in a steam environment. After the sodium hydroxide added in the corn cob pretreatment process plays the function of the catalyst, the sodium hydroxide continues to be used as a reaction raw material to participate in the production process of the sodium humate, so that the waste and the recycling investment of the catalyst are avoided. 4. The product simultaneously contains xylo-oligosaccharide and sodium humate, and the xylo-oligosaccharide promotes the growth of beneficial bacteria and inhibits the proliferation of harmful bacteria; the sodium humate further removes toxins secreted by harmful bacteria, and the two have synergistic effect to promote healthy development of intestinal tracts. 5. The production process combines the processes of centrifugation, precipitation and roller drying, so that the water-insoluble substances are removed to the maximum extent, and the product quality is improved. 6. The drying process adopts roller drying, and the product does not need crushing treatment, reduces the influence of dust on the environment in the production process.
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FIG. 1 is a process flow diagram of the present invention.
Detailed Description
Example 1: a sodium humate product containing oligosaccharide comprises the following components in parts by weight: 25 parts of corncobs, 55 parts of humic acid and 15 parts of sodium hydroxide.
The preparation method of the oligosaccharide-containing sodium humate product comprises the following steps: 1. adding 25 parts of corncobs and 5 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 150 ℃, stirring for reaction for 1.5 hours, standing and cooling to obtain cellulose and hemicellulose.
2. Adding 55 parts of humic acid mineral powder crushed to 80 meshes into a reaction kettle, controlling the temperature to be 105 ℃, stirring and reacting for 1 hour to obtain xylooligosaccharide, glucose oligosaccharide and a small amount of sodium humate, standing and cooling.
3. Adding 10 parts of sodium hydroxide into a reaction kettle, controlling the temperature at 70 ℃, stirring and reacting for 2 hours to obtain oligosaccharide and sodium humate, standing and cooling.
4. The reaction solution was centrifuged for 0.5 hour to obtain a centrifuged solution.
5. Placing the centrifugate in a drying sedimentation tank, standing for 6 hours, and drying in a roller.
6. And (3) sieving the obtained product by a 20-mesh sieve to obtain a sodium humate product containing oligosaccharide, sampling and detecting, wherein 8.3% of oligosaccharide, 55.4% of humic acid and 6.9% of water-insoluble substances are packaged and warehoused after being detected to be qualified.
Example 2: a sodium humate product containing oligosaccharide comprises the following components in parts by weight: 28 parts of corncobs, 58 parts of humic acid and 15 parts of sodium hydroxide.
The preparation method of the oligosaccharide-containing sodium humate product comprises the following steps: 1. adding 28 parts of corncobs and 7 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 170 ℃, stirring for reaction for 1 hour, standing and cooling to obtain cellulose and hemicellulose.
2. And adding 58 parts of humic acid mineral powder crushed to 80 meshes into a reaction kettle, controlling the temperature to be 110 ℃, stirring and reacting for 1.5 hours to obtain xylooligosaccharide, glucose oligosaccharide and a small amount of sodium humate, standing and cooling.
3. Adding 8 parts of sodium hydroxide into a reaction kettle, controlling the temperature to be 80 ℃, stirring and reacting for 3 hours to obtain oligosaccharide and sodium humate, standing and cooling.
4. The reaction solution was centrifuged for 0.5 hour to obtain a centrifuged solution.
5. Placing the centrifugate in a drying sedimentation tank, standing for 7 hours, and drying in a roller.
6. And (3) sieving the obtained product by a 20-mesh sieve to obtain a sodium humate product containing oligosaccharide, sampling and detecting, wherein the content of oligosaccharide is 9.4%, the content of humic acid is 57.3%, and the content of water-insoluble substances is 5.4%, and packaging and warehousing after the detection is qualified.
Example 3: a sodium humate product containing oligosaccharide comprises the following components in parts by weight: 30 parts of corncobs, 60 parts of humic acid and 15 parts of sodium hydroxide.
The preparation method of the oligosaccharide-containing sodium humate product comprises the following steps: 1. adding 30 parts of corncobs and 10 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 180 ℃, stirring for reaction for 3 hours, standing and cooling to obtain cellulose and hemicellulose.
2. Adding 60 parts of humic acid mineral powder crushed to 80 meshes into a reaction kettle, controlling the temperature at 120 ℃, stirring and reacting for 2 hours to obtain xylooligosaccharide, glucose oligosaccharide and a small amount of sodium humate, standing and cooling.
3. Adding 5 parts of sodium hydroxide into a reaction kettle, controlling the temperature to be 90 ℃, stirring and reacting for 4 hours to obtain oligosaccharide and sodium humate, standing and cooling.
4. The reaction solution was centrifuged for 0.5 hour to obtain a centrifuged solution.
5. Placing the centrifugate in a drying sedimentation tank, standing for 10 hours, and drying in a roller.
6. And (3) sieving the obtained product by a 20-mesh sieve to obtain a sodium humate product containing oligosaccharide, sampling and detecting, wherein 10.7% of oligosaccharide, 60.2% of humic acid and 5.1% of water-insoluble substances are packaged and warehoused after being detected to be qualified.
Example 4: a sodium humate product containing oligosaccharide comprises the following components in parts by weight: 30 parts of corncobs, 60 parts of humic acid and 15 parts of sodium hydroxide.
The preparation method of the oligosaccharide-containing sodium humate product comprises the following steps:
1. adding 30 parts of corncobs and 10 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 100 ℃, stirring for reaction for 3 hours, standing and cooling.
2. Adding 60 parts of humic acid mineral powder crushed to 80 meshes into a reaction kettle, controlling the temperature to be 120 ℃, stirring for reaction for 2 hours, standing and cooling. 3. Adding 5 parts of sodium hydroxide into a reaction kettle, controlling the temperature to be 50 ℃, stirring for reaction for 4 hours, standing and cooling. 4. Centrifuging the reaction solution for 0.5 hour; 5. placing the centrifugate in a drying sedimentation tank, standing for 10 hours, and drying in a roller. 6. And (3) sieving the obtained product by a 20-mesh sieve to obtain a sodium humate product containing oligosaccharide, and sampling and detecting to obtain 2.6% of oligosaccharide, 32.3% of humic acid and 5.4% of water-insoluble substances, wherein the content of humic acid is not less than 55% of that required by a single feed raw material, and the product is unqualified.
Example 5: the application of the product containing oligosaccharide sodium humate as feed additive for livestock and poultry breeding can reduce diarrhea and promote pig growth.
Mixing the product containing oligosaccharide sodium humate with feed at a ratio of 0.3%, and directly feeding livestock and fowl.
The test process comprises the following steps: the experimental subject is a certain commercial pork pig, and 200 pigs are used in each group.
Control group: daily ration, nutrient components, feeding management and the like are carried out according to the conventional method of a pig farm.
Experimental groups: the feed was supplemented with the oligosaccharide sodium humate-containing preparation obtained in example 3, and the other daily rations, nutrients and feeding management were the same as those of the control group.
The test results are shown in table 1:
the results show that: compared with a control group, the sodium humate containing oligosaccharide can reduce the diarrhea rate, effectively improve the growth rate of commercial pigs, reduce the feed-meat ratio, and reduce the feed-meat ratio by 0.06.
Example 6: application of oligosaccharide-containing sodium humate product in promotion of intestinal development of broiler chickens
1. The sodium humate product containing oligosaccharide obtained in example 3 was mixed with feed at a ratio of 0.3% and fed directly.
2. The test process comprises the following steps: the experimental subjects were broilers in a commercial broiler farm, and each group contained 600 broilers.
Control group: daily ration, nutrient components, feeding management and the like are carried out according to the conventional method of a pig farm.
Experimental groups: the feed is added with 0.3% of oligosaccharide-containing sodium humate preparation, and other daily rations, nutrient components and feeding management are the same as those of a control group.
The results show that: compared with the control group, the broiler chickens in the experimental group can promote intestinal villus development, improve villus length/crypt value and enhance intestinal health and nutrient absorption capacity by adding the sodium humate containing oligosaccharide.
Example 7: application of oligosaccharide-containing sodium humate product in promotion of intestinal development of broiler chickens
1. The sodium humate product containing oligosaccharide obtained in example 4 and feed were mixed in proportions of 0.3%, 0.6% and 1.2%, respectively, and fed directly.
2. The test process comprises the following steps: the experimental subjects were broilers in a commercial broiler farm, and each group contained 600 broilers.
Control group: the daily ration, nutrient components, feeding management and the like are carried out according to the conventional method of a chicken farm.
Experimental group 1: the feed is added with 0.3% of oligosaccharide-containing sodium humate preparation, and other daily rations, nutrient components and feeding management are the same as those of a control group.
Experimental group 2: the feed is added with 0.6% of the preparation containing oligosaccharide sodium humate, and other daily rations, nutrient components and feeding management are the same as those of a control group.
Experimental group 3: 1.2% of the preparation containing oligosaccharide sodium humate is added into the feed, and other daily rations, nutrient components and feeding management are the same as those of a control group.
The results show that: compared with the control group, the broiler chickens in the experimental group have almost no influence on the development of intestinal villus when 0.3 percent of oligosaccharide-containing sodium humate is added; when 0.6 percent of the additive is added, the additive has certain promotion effect on intestinal villus development, but the effect is obviously lower than that of the sample addition group in the example 3; when the addition amount is increased to 1.2%, the intestinal villus development level is obviously reduced, which shows that the excessive addition amount has an inhibition effect on the intestinal development.
Claims (4)
1. A sodium humate product containing oligosaccharide is characterized by being prepared from the following components in parts by weight: 25-30 parts of corncobs, 55-60 parts of humic acid mineral powder and 10-15 parts of sodium hydroxide;
the preparation method of the oligosaccharide-containing sodium humate product comprises the following steps:
(1) adding 25-30 parts of corncobs and 5-10 parts of sodium hydroxide into a reaction kettle; introducing steam, controlling the temperature at 150-; (2) adding 55-60 parts of humic acid mineral powder crushed to 60-100 meshes into a reaction kettle; introducing steam, controlling the temperature at 105-120 ℃, stirring and reacting for 1-2 hours to obtain xylo-oligosaccharide, glucose oligosaccharide and a small amount of sodium humate, standing and cooling; (3) adding 5-10 parts of sodium hydroxide into the reaction kettle in the step (2), controlling the temperature to be 70-90 ℃, stirring and reacting for 2-4 hours to obtain oligosaccharide and sodium humate, standing and cooling; (4) centrifuging the reaction solution for 0.5 hour to obtain a centrifugate; (5) placing the centrifugate in a drying sedimentation tank, standing for 6-10 hours, and taking supernatant; (6) drying the supernatant in a roller to obtain flaky particles; the sodium humate product dried by the roller is black; sieving the flaky particles with a 16-20 mesh sieve; thus obtaining the product containing oligosaccharide sodium humate.
2. The sodium humate product containing oligosaccharide as claimed in claim 1, wherein the product comprises 30 parts of corncob, 60 parts of humic acid mineral powder and 15 parts of sodium hydroxide.
3. The use of the sodium humate product containing oligosaccharides as defined in claim 1, wherein the sodium humate product containing oligosaccharides is used as a feed additive in livestock breeding.
4. The application of the sodium humate product containing oligosaccharide as claimed in claim 3, wherein the sodium humate product containing oligosaccharide is mixed with feed at a ratio of 0.3% for direct feeding to livestock and poultry.
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