CN114246260A - Feed additive and preparation method thereof - Google Patents
Feed additive and preparation method thereof Download PDFInfo
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- CN114246260A CN114246260A CN202111508945.0A CN202111508945A CN114246260A CN 114246260 A CN114246260 A CN 114246260A CN 202111508945 A CN202111508945 A CN 202111508945A CN 114246260 A CN114246260 A CN 114246260A
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- feed additive
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- hydroxyacetophenone
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- 239000003674 animal food additive Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- TXFPEBPIARQUIG-UHFFFAOYSA-N 4'-hydroxyacetophenone Chemical compound CC(=O)C1=CC=C(O)C=C1 TXFPEBPIARQUIG-UHFFFAOYSA-N 0.000 claims abstract description 58
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- LAZPBGZRMVRFKY-HNCPQSOCSA-N Levamisole hydrochloride Chemical compound Cl.C1([C@H]2CN3CCSC3=N2)=CC=CC=C1 LAZPBGZRMVRFKY-HNCPQSOCSA-N 0.000 claims abstract description 21
- 229960003734 levamisole hydrochloride Drugs 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 19
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012346 acetyl chloride Substances 0.000 claims abstract description 16
- 230000010933 acylation Effects 0.000 claims abstract description 16
- 238000005917 acylation reaction Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 239000012046 mixed solvent Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 12
- 150000003751 zinc Chemical class 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 18
- INVGWHRKADIJHF-UHFFFAOYSA-N Sanguinarin Chemical compound C1=C2OCOC2=CC2=C3[N+](C)=CC4=C(OCO5)C5=CC=C4C3=CC=C21 INVGWHRKADIJHF-UHFFFAOYSA-N 0.000 claims description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 10
- 239000002808 molecular sieve Substances 0.000 claims description 10
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 10
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- FCEXWTOTHXCQCQ-UHFFFAOYSA-N Ethoxydihydrosanguinarine Natural products C12=CC=C3OCOC3=C2C(OCC)N(C)C(C2=C3)=C1C=CC2=CC1=C3OCO1 FCEXWTOTHXCQCQ-UHFFFAOYSA-N 0.000 claims description 6
- IPMYMEWFZKHGAX-UHFFFAOYSA-N Isotheaflavin Natural products OC1CC2=C(O)C=C(O)C=C2OC1C(C1=C2)=CC(O)=C(O)C1=C(O)C(=O)C=C2C1C(O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-UHFFFAOYSA-N 0.000 claims description 6
- UXRMWRBWCAGDQB-UHFFFAOYSA-N Theaflavin Natural products C1=CC(C2C(CC3=C(O)C=C(O)C=C3O2)O)=C(O)C(=O)C2=C1C(C1OC3=CC(O)=CC(O)=C3CC1O)=CC(O)=C2O UXRMWRBWCAGDQB-UHFFFAOYSA-N 0.000 claims description 6
- 229940084560 sanguinarine Drugs 0.000 claims description 6
- YZRQUTZNTDAYPJ-UHFFFAOYSA-N sanguinarine pseudobase Natural products C1=C2OCOC2=CC2=C3N(C)C(O)C4=C(OCO5)C5=CC=C4C3=CC=C21 YZRQUTZNTDAYPJ-UHFFFAOYSA-N 0.000 claims description 6
- IPMYMEWFZKHGAX-ZKSIBHASSA-N theaflavin Chemical compound C1=C2C([C@H]3OC4=CC(O)=CC(O)=C4C[C@H]3O)=CC(O)=C(O)C2=C(O)C(=O)C=C1[C@@H]1[C@H](O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-ZKSIBHASSA-N 0.000 claims description 6
- 229940026509 theaflavin Drugs 0.000 claims description 6
- 235000014620 theaflavin Nutrition 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 241001465754 Metazoa Species 0.000 abstract description 11
- 239000000654 additive Substances 0.000 abstract description 6
- 230000000996 additive effect Effects 0.000 abstract description 5
- 241000894006 Bacteria Species 0.000 abstract description 4
- 230000036039 immunity Effects 0.000 abstract description 3
- 235000016709 nutrition Nutrition 0.000 abstract description 2
- 230000035764 nutrition Effects 0.000 abstract description 2
- 230000037396 body weight Effects 0.000 description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000009395 breeding Methods 0.000 description 2
- 230000001488 breeding effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 241000287828 Gallus gallus Species 0.000 description 1
- HLFSDGLLUJUHTE-SNVBAGLBSA-N Levamisole Chemical compound C1([C@H]2CN3CCSC3=N2)=CC=CC=C1 HLFSDGLLUJUHTE-SNVBAGLBSA-N 0.000 description 1
- 241000282887 Suidae Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 235000013330 chicken meat Nutrition 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 229960001614 levamisole Drugs 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/30—Oligoelements
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/116—Heterocyclic compounds
- A23K20/121—Heterocyclic compounds containing oxygen or sulfur as hetero atom
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/116—Heterocyclic compounds
- A23K20/137—Heterocyclic compounds containing two hetero atoms, of which at least one is nitrogen
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/70—Feeding-stuffs specially adapted for particular animals for birds
- A23K50/75—Feeding-stuffs specially adapted for particular animals for birds for poultry
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/06—Zinc compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Organic Chemistry (AREA)
- Birds (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a feed additive and a preparation method thereof, wherein the preparation method comprises the following steps: putting phenol and a catalyst into an acylation kettle, heating to 45-55 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle not more than 120 ℃ in the dropwise adding process, preserving heat for 7-10 hours after dropwise adding is finished, and cooling to obtain a material A; hydrolyzing the material A, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone; adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water for uniform dispersion, and adding zinc salt for uniform dispersion to obtain a material B; and (3) placing the material B in a hydrothermal reaction kettle for hydrothermal reaction, cooling to room temperature after the reaction is finished, filtering, washing and drying to obtain the feed additive. The preparation method of the feed additive provided by the invention is simple in process, and the obtained additive can provide nutrition for animals, and simultaneously can resist bacteria, improve immunity and promote growth of the animals.
Description
Technical Field
The invention relates to the technical field of synthesis, in particular to a feed additive and a preparation method thereof.
Background
The feed additive is a small amount or trace substance added in the production, processing and using processes of the feed, has a small dosage in the feed but an obvious effect, and has obvious effects on enhancing the nutritive value of basic feed, improving the production performance of animals, ensuring the health of the animals, saving the cost of the feed, improving the quality of products and the like. In recent years, with the development of the breeding industry, various feed additives appear, the breeding level and the benefit are improved, but some feed additives have single effect after being used, the weight increasing effect is not ideal, and the application of the feed additives is limited.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the feed additive and the preparation method thereof, the preparation method is simple in process, and the obtained additive can provide nutrition for animals, and simultaneously can resist bacteria, improve immunity and promote growth of the animals.
The invention provides a preparation method of a feed additive, which comprises the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 45-55 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle not more than 120 ℃ in the dropwise adding process, preserving heat for 7-10 hours after dropwise adding is completed, and cooling to obtain a material A;
s2, hydrolyzing the material A, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water for uniform dispersion, and adding zinc salt for uniform dispersion to obtain a material B;
s4, placing the material B in a hydrothermal reaction kettle for hydrothermal reaction, cooling to room temperature after the reaction is finished, filtering, washing and drying to obtain the feed additive.
Preferably, in S1, the catalyst is a mixture of aluminum trichloride, trifluoromethanesulfonic acid, and beta molecular sieve.
Preferably, in S1, the catalyst is aluminum trichloride, trifluoromethanesulfonic acid, and a beta molecular sieve in a weight ratio of 10-25: 1-3: 2-5.
Preferably, in S1, the molar mass ratio of the phenol, the catalyst and the acetyl chloride is 1 mol: 1-5 g: 1-1.1 mol.
Preferably, in S2, the temperature of the hydrolysis is 25-35 ℃.
Preferably, in S3, the molar ratio of the p-hydroxyacetophenone, the levamisole hydrochloride and the zinc salt is 1: 1: 1-3.
Preferably, in S3, the zinc salt is one or more of zinc nitrate, zinc sulfate, zinc acetate and zinc chloride; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 1-5.
Preferably, in S4, the temperature of the hydrothermal reaction is 120-145 ℃ and the time is 50-75 h.
Preferably, in S4, the method further comprises mixing the dried product with theaflavin and sanguinarine in a ratio of 10-20: 1-4: 2-9 weight ratio.
The invention also provides a feed additive, which is prepared by adopting the preparation method of the feed additive.
In the preparation method of the feed additive, phenol and acetyl chloride are used as raw materials, and are reacted under the action of a catalyst, and the reaction process is controlled to obtain p-hydroxyacetophenone; then, the obtained p-hydroxyacetophenone and levamisole hydrochloride are taken as ligands, a mixed solvent of ethanol and water is taken as a solvent, zinc salt is taken as metal salt to carry out hydrothermal reaction, so that oxygen and nitrogen atoms in the p-hydroxyacetophenone and the levamisole hydrochloride are coordinated with zinc, and the feed additive is obtained, and combines the p-hydroxyacetophenone, the levamisole hydrochloride and the zinc into a whole, so that on one hand, nutrients such as zinc element and the like can be provided for animals, the appetite of the animals is enhanced, the growth of the animals is promoted, on the other hand, microorganisms can be resisted, the growth of harmful bacteria is inhibited, intestinal flora is kept normal, the morbidity is reduced, and the utilization rate of the feed is improved; in a preferred mode, when the p-hydroxyacetophenone is prepared, a mixture of aluminum trichloride, trifluoromethanesulfonic acid and a beta molecular sieve is specifically selected as a catalyst, the catalytic performance is excellent, the obtained p-hydroxyacetophenone has high yield and good purity, the yield reaches more than 97.8%, and the purity is more than 99.6%; the obtained complex is further mixed with theaflavin and sanguinarine according to the weight ratio of 10-20: 1-4: 2-9, so that the three components play excellent synergistic action, can stimulate immune system cells in intestinal tracts while resisting bacteria, improve the immunity of animals and promote the growth of the animals.
The preparation method of the feed additive has the advantages of simple process, easy control, high yield of more than 93.8 percent, good purity of more than 98.9 percent and stable product; when the feed is fed to pigs for 30 days, compared with the feed without the additive, the pig skin hair red brightness is improved by 6-12%, the daily gain is improved by 8-15%, and the feed conversion rate is improved by more than 14%.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
The invention provides a preparation method of a feed additive, which comprises the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 55 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle not more than 120 ℃ in the dropwise adding process, preserving heat for 10 hours after dropwise adding is completed, and cooling to obtain a material A; wherein the molar mass ratio of the phenol to the catalyst to the acetyl chloride is 1 mol: 1 g: 1.1 mol; the catalyst is aluminum trichloride, trifluoromethanesulfonic acid and a beta molecular sieve in a weight ratio of 10: 3: 2;
s2, hydrolyzing the material A at 25 ℃, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water, uniformly dispersing, adding zinc nitrate, and uniformly dispersing to obtain a material B; wherein the mol ratio of the p-hydroxyacetophenone to the levamisole hydrochloride to the zinc nitrate is 1: 1: 2; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 3;
s4, placing the material B in a hydrothermal reaction kettle, carrying out hydrothermal reaction at 120 ℃ for 75h, cooling to room temperature after the reaction is finished, filtering, washing and drying to obtain the feed additive.
Example 2
The invention provides a preparation method of a feed additive, which comprises the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 45 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle at 110 ℃ in the dropwise adding process, preserving heat for 9 hours after dropwise adding is finished, and cooling to obtain a material A; wherein the molar mass ratio of the phenol to the catalyst to the acetyl chloride is 1 mol: 1.5 g: 1 mol; the catalyst is aluminum trichloride, trifluoromethanesulfonic acid and a beta molecular sieve in a weight ratio of 25: 1: 5 with a mixture of;
s2, hydrolyzing the material A at 30 ℃, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water, uniformly dispersing, adding zinc sulfate, and uniformly dispersing to obtain a material B; wherein the mol ratio of the p-hydroxyacetophenone to the levamisole hydrochloride to the zinc sulfate is 1: 1: 3; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 1;
s4, placing the material B in a hydrothermal reaction kettle, carrying out hydrothermal reaction for 50h at 145 ℃, cooling to room temperature after the reaction is finished, filtering, washing and drying to obtain the feed additive.
Example 3
The invention provides a preparation method of a feed additive, which comprises the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 52 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle at 115 ℃ in the dropwise adding process, preserving heat for 7 hours after dropwise adding is finished, and cooling to obtain a material A; wherein the molar mass ratio of the phenol to the catalyst to the acetyl chloride is 1 mol: 5 g: 1 mol; the catalyst is aluminum trichloride, trifluoromethanesulfonic acid and a beta molecular sieve in a weight ratio of 10: 2: 3;
s2, hydrolyzing the material A at 35 ℃, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water for uniform dispersion, and adding zinc salt for uniform dispersion to obtain a material B; wherein the mol ratio of the p-hydroxyacetophenone to the levamisole hydrochloride to the zinc salt is 1: 1: 1; the zinc salt is zinc nitrate and zinc chloride, and the weight ratio of the zinc salt to the zinc chloride is 1: 1; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 1;
s4, placing the material B in a hydrothermal reaction kettle, carrying out hydrothermal reaction for 60 hours at 125 ℃, cooling to room temperature after the reaction is finished, filtering, washing, drying, mixing with theaflavin and sanguinarine according to the weight ratio of 10: 4: 9 to obtain the feed additive.
Example 4
The invention provides a preparation method of a feed additive, which comprises the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 48 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle at 120 ℃ in the dropwise adding process, preserving the heat for 7.5 hours after the dropwise adding is finished, and cooling to obtain a material A; wherein the molar mass ratio of the phenol to the catalyst to the acetyl chloride is 1 mol: 1 g: 1 mol; the catalyst is aluminum trichloride, trifluoromethanesulfonic acid and a beta molecular sieve in a weight ratio of 14: 1: 3.5 of a mixture;
s2, hydrolyzing the material A at 28 ℃, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water, uniformly dispersing, adding zinc nitrate, and uniformly dispersing to obtain a material B; wherein the mol ratio of the p-hydroxyacetophenone to the levamisole hydrochloride to the zinc nitrate is 1: 1: 1.6; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 4;
s4, placing the material B in a hydrothermal reaction kettle, carrying out hydrothermal reaction at 130 ℃ for 55h, cooling to room temperature after the reaction is finished, filtering, washing and drying, and mixing the obtained product with theaflavin and sanguinarine according to the weight ratio of 20: 1: 2 to obtain the feed additive.
Example 5
The invention provides a preparation method of a feed additive, which comprises the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 50 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle at 110 ℃ in the dropwise adding process, preserving the heat for 8 hours after the dropwise adding is finished, and cooling to obtain a material A; wherein the molar mass ratio of the phenol to the catalyst to the acetyl chloride is 1 mol: 2.6 g: 1.1 mol; the catalyst is aluminum trichloride, trifluoromethanesulfonic acid and a beta molecular sieve in a weight ratio of 10: 1: 2;
s2, hydrolyzing the material A at 28 ℃, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water, uniformly dispersing, adding zinc nitrate, and uniformly dispersing to obtain a material B; wherein the mol ratio of the p-hydroxyacetophenone to the levamisole hydrochloride to the zinc nitrate is 1: 1: 1.5; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 2;
s4, placing the material B in a hydrothermal reaction kettle, carrying out hydrothermal reaction at 135 ℃ for 72h, cooling to room temperature after the reaction is finished, filtering, washing and drying, and mixing the obtained product with theaflavin and sanguinarine according to the weight ratio of 15: 2: 7 to obtain the feed additive.
Selecting 210 healthy chicks of 30 days old for testing, and randomly dividing the chicks into 7 groups of 30 chicks each; wherein 1 group is blank control group, 1 group is levamisole hydrochloride control group, and the rest 5 groups are used as test groups and respectively adopt the additives in the embodiments 1-5; when levamisole hydrochloride and the additive are fed, the levamisole hydrochloride and the additive are added according to the addition amount of 6mg per kilogram of body weight, and the addition is continuously carried out for 3 days; after feeding is finished for 7d, 14d and 21d, randomly extracting 10 chickens from each group, and weighing on empty stomach; the blank control group is weighed to obtain the initial average body weight of 225.8g, the average body weight of 366.9g after 7d, the average body weight of 492.3g after 14d and the average body weight of 602.5g after 21 d; the initial body weight of the levamisole control group is 210.9g, the average body weight after 7 days is 396.7g, the average body weight after 14 days is 496.9g, and the average body weight after 21 days is 594.5 g; in the test groups of examples 1 to 5, the initial average body weight was 204.1 to 209.7g, the average body weight was 422.0 to 463.1g after 7 days, the average body weight was 538.2 to 557.8g after 14 days, and the average body weight was 659.3 to 678.4g after 21 days.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The preparation method of the feed additive is characterized by comprising the following steps:
s1, putting phenol and a catalyst into an acylation kettle, heating to 45-55 ℃, dropwise adding acetyl chloride under negative pressure, keeping the temperature in the acylation kettle not more than 120 ℃ in the dropwise adding process, preserving heat for 7-10 hours after dropwise adding is completed, and cooling to obtain a material A;
s2, hydrolyzing the material A, washing with water, separating a water layer, distilling, freezing, crystallizing and centrifuging to obtain p-hydroxyacetophenone;
s3, adding p-hydroxyacetophenone and levamisole hydrochloride into a mixed solvent of ethanol and water for uniform dispersion, and adding zinc salt for uniform dispersion to obtain a material B;
s4, placing the material B in a hydrothermal reaction kettle for hydrothermal reaction, cooling to room temperature after the reaction is finished, filtering, washing and drying to obtain the feed additive.
2. The method for preparing feed additive according to claim 1, wherein in S1, the catalyst is a mixture of aluminum trichloride, trifluoromethanesulfonic acid and beta-molecular sieve.
3. The method for preparing the feed additive according to claim 1, wherein in S1, the catalyst is aluminum trichloride, trifluoromethanesulfonic acid, beta molecular sieve in a weight ratio of 10-25: 1-3: 2-5.
4. The method for preparing feed additive according to claim 1, wherein in S1, the molar mass ratio of the phenol, the catalyst and the acetyl chloride is 1 mol: 1-5 g: 1-1.1 mol.
5. The method for preparing a feed additive according to claim 1, wherein the hydrolysis temperature is 25-35 ℃ in S2.
6. The method for preparing feed additive according to claim 1, wherein the molar ratio of p-hydroxyacetophenone, levamisole hydrochloride and zinc salt in S3 is 1: 1: 1-3.
7. The method for preparing feed additive according to claim 1, wherein in S3, the zinc salt is one or more of zinc nitrate, zinc sulfate, zinc acetate and zinc chloride; in the mixed solvent of ethanol and water, the volume ratio of ethanol to water is 1: 1-5.
8. The method for preparing feed additive according to claim 1, wherein the hydrothermal reaction is performed at a temperature of 120-145 ℃ for 50-75h in S4.
9. The method for preparing a feed additive according to any one of claims 1 to 8, wherein in S4, the method further comprises mixing the dried product with theaflavin and sanguinarine in a ratio of 10 to 20: 1-4: 2-9 weight ratio.
10. A feed additive, which is prepared by the method for preparing a feed additive according to any one of claims 1 to 9.
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| CN202111508945.0A CN114246260A (en) | 2021-12-10 | 2021-12-10 | Feed additive and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106167449A (en) * | 2016-07-24 | 2016-11-30 | 遵义师范学院 | A kind of synthetic method of parahydroxyacet-ophenone |
| CN106916060A (en) * | 2017-02-22 | 2017-07-04 | 江苏新瀚新材料股份有限公司 | A kind of preparation method of high-purity parahydroxyacet-ophenone |
| CN107624980A (en) * | 2017-10-17 | 2018-01-26 | 天津市美农动物科技有限公司 | A kind of boar health-care feed and preparation method thereof |
| CN113729121A (en) * | 2021-08-27 | 2021-12-03 | 山东雨田食品科技股份有限公司 | Feed additive containing zinc benzoate and production process and application thereof |
-
2021
- 2021-12-10 CN CN202111508945.0A patent/CN114246260A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106167449A (en) * | 2016-07-24 | 2016-11-30 | 遵义师范学院 | A kind of synthetic method of parahydroxyacet-ophenone |
| CN106916060A (en) * | 2017-02-22 | 2017-07-04 | 江苏新瀚新材料股份有限公司 | A kind of preparation method of high-purity parahydroxyacet-ophenone |
| CN107624980A (en) * | 2017-10-17 | 2018-01-26 | 天津市美农动物科技有限公司 | A kind of boar health-care feed and preparation method thereof |
| CN113729121A (en) * | 2021-08-27 | 2021-12-03 | 山东雨田食品科技股份有限公司 | Feed additive containing zinc benzoate and production process and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郭洋 等: "盐酸左旋咪唑对雏鸡免疫功能及生长性能影响的研究" * |
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