CN104351483A - Preparation method of completely fermented oxytetracycline calcium granules - Google Patents
Preparation method of completely fermented oxytetracycline calcium granules Download PDFInfo
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- CN104351483A CN104351483A CN201410648072.7A CN201410648072A CN104351483A CN 104351483 A CN104351483 A CN 104351483A CN 201410648072 A CN201410648072 A CN 201410648072A CN 104351483 A CN104351483 A CN 104351483A
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Abstract
The invention discloses a preparation method of completely fermented oxytetracycline calcium granules. By taking oxytetracycline fermentation liquor as an initiating raw material, the preparation method is used for preparing granules of the oxytetracycline calcium by virtue of steps of calcifying an oxytetracycline fermentation liquor as a raw material, acidizing, filtering, crushing, pelletizing, straightening, drying and sieving. The preparation method disclosed by the invention can be used for overcoming the defects that a conventional spray drying process is high in energy consumption and not environmentally-friendly, and the completely fermented oxytetracycline calcium granules obtained by adopting a conventional method have the defect of inconvenience in use. The oxytetracycline calcium granules prepared by adopting the preparation method disclosed by the invention is uniform, compact, beautiful, good in mobility, unlikely to crush, convenient to use and capable of meeting the needs of a client very well.
Description
Technical field
The invention belongs to field of feed additive technology, relate to a kind of preparation method of feed addictive, be specifically related to a kind of preparation method of full fermentation oxytetracycline calcium particle.
Background technology
Terramycin (Oxytetracycline) is the one of TCs, antibacterial action is had to most gram positive bacteria, negative bacterium, coccus and bacillus, also having inhibitory action to Richettsia and amcbiasis protozoon, is the antibiotic feed additive with growth promoting effects and disease preventing and treating in the feed extensively making an addition to children pig in age, chicken, ox and Adult Chicken etc.But terramycin directly applies to feed interpolation can affect animal to calcareous absorption, and oxytetracycline calcium can play the somatotrophic effect of sterilization on the one hand, on the other hand can to supplement needed for health calcareous for domestic animal, simultaneously for raising terramycin stability and long-lastingly also have positive effect.Therefore be widely applied in feed additive industry for animals.
The nineties in last century, the Li Yongchang etc. of Heilungkiang biological products two factory have studied " the feeding oxytetracycline calcium of full fermentation " technique, and adopt spray drying device to prepare oxytetracycline calcium, this technique is used till today always.This technique adopts steam and electric power, and evaporated by moisture, power consumption is high; Product appearance is Powdered, and poor fluidity, has dust from flying during use, and not easily mixes thoroughly with feed, uses very inconvenient.
In order to meet the demand of feed additive industry to oxytetracycline calcium product quality, being the call of response national energy-saving environmental protection simultaneously, being necessary the preparation method of the oxytetracycline calcium developing a kind of energy-conserving and environment-protective, to obtain good fluidity, oxytetracycline calcium easy to use.
Summary of the invention
The object of this invention is to provide a kind of preparation method of oxytetracycline calcium of energy-conserving and environment-protective, the oxytetracycline calcium good fluidity that the method prepares, easy to use, the demand of feed additive industry can be met.
In order to realize object of the present invention, inventor provide following technical scheme.
A preparation method for full fermentation oxytetracycline calcium particle, comprises the following steps:
A. in Performance in Oxytetracycline Fermentation Broth, add calcium carbonate, stir, reaction 1-5h, obtains the calcifying solution of terramycin;
Add hydrochloric acid in the calcifying solution of the terramycin b. obtained to step a, the pH value regulating calcifying solution is 4.5-6.5, obtains acidifying solution;
C. the acidifying solution that step b obtains is pumped into autoclave diaphragm sheet frame to filter, the moisture squeezed to filter cake is 40-50%, obtains the filter cake of oxytetracycline calcium;
The filter cake wet stock pulverizer of the oxytetracycline calcium d. obtained by step c is pulverized, and obtains oxytetracycline calcium wet-milling;
E. oxytetracycline calcium wet-milling steps d obtained directly is granulated, whole grain, drying, screening, namely obtain the particle of oxytetracycline calcium.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, the addition of calcium carbonate described in step a is 0.7-0.9 times of contained terramycin amount in Performance in Oxytetracycline Fermentation Broth, and preferred 0.75-0.8 doubly.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, the time of reacting described in step a preferred 2h.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, the concentration of hydrochloric acid described in step b is 1N.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, regulates the preferred 5.0-5.5 of the pH value of calcifying solution described in step b.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, during the plate-frame filtering of autoclave diaphragm described in step c, squeeze pressure is 1-1.5Mpa.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, the moisture squeezed described in step c to filter cake is 45%.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, carries out the grinding particle size≤1mm pulverized with wet stock pulverizer described in steps d.
The preparation method of above-mentioned full fermentation oxytetracycline calcium particle, the particle diameter of directly granulating described in step e is 0.6-1.2mm, and described screening sieve number is 10-100 order, namely gets the lower particle of 10 mesh sieve sieve after 100 mesh sieves, gets the upper particle of sieve.
In described preparation method; step e directly granulates and rotary squeezing granulator or oscillating granulator can be selected to carry out; then whole grain is carried out with shot-blasting machine; select vibrated fluidized bed subsequently or fluidizing fluid-bedly carry out drying; time dry, EAT controls as 170-200 DEG C, and leaving air temp controls, for 85-100 DEG C, finally dried particle spin vibration sieve or square sieve to be sieved; namely obtain the particle of oxytetracycline calcium, can be used as feed addictive and use.The preferred rotary squeezing granulator of facility for granulating; the preferred 0.6mm of particle diameter that namely aperture of granulator screen cloth granulates; the preferred vibrated fluidized bed of drying equipment; EAT preferred 170-180 DEG C time dry, the preferred 85-90 DEG C of leaving air temp, the preferred square sieve of screening plant; the preferred 20-80 order of sieve number; gained particle is more even, uses more convenient, more easily mixes thoroughly after interpolation.
The preparation method of oxytetracycline calcium particle provided by the present invention is applicable to terramycin prepared by full fermentation, initiation material is Performance in Oxytetracycline Fermentation Broth, namely by be full of cracks Streptothrix through three grade fermemtation gained zymotic fluid, main component is terramycin, also comprises the impurity such as be full of cracks Streptothrix mycelium, remaining culture medium.In zymotic fluid, the concentration unit of terramycin is generally 32000-36000u/ml.
The present invention adopts autoclave diaphragm plate-frame filtering to obtain the wet solid material of oxytetracycline calcium, terramycin is filtered in filter cake together with mycelium, remaining medium protein, solve the environmental issue of bacterium Slag treatment, and substantial saving in the energy, the energy-conservation 5-6 of more traditional spray drying process doubly, and simple to operate, be easy to control, there is good promotional value.
In preparation method of the present invention, the dry run of oxytetracycline calcium particle is heated evenly, and heated time is short, and product quality is more stable.
The oxytetracycline calcium uniform particles that the present invention prepares, solid, attractive in appearance, good fluidity, not easily fragmentation, easy to use, the demand of client can be better met.
Detailed description of the invention
Below in conjunction with specific embodiment, content of the present invention is further described in detail.
Embodiment 1
Measure 30l Performance in Oxytetracycline Fermentation Broth, detection fermentation unit is 34152u/ml, adds calcium carbonate 0.8kg wherein, stirs 2h, carries out calcify reaction; In terramycin calcifying solution, add 1N hydrochloric acid carry out acidifying, regulate calcifying solution pH to 5.5; Acidifying liquid is pumped into autoclave diaphragm plate-frame filtering, pressure 1.5Mpa, squeezing to moisture content is 45%, obtains oxytetracycline calcium wet cake; Pulverized by oxytetracycline calcium wet cake wet stock pulverizer, grinding particle size 0.8mm, makes it dispersed; Oxytetracycline calcium wet powder is passed into rotary squeezing granulator (particle diameter 0.6mm) screen cloth to granulate; whole grain 20min is carried out with shot-blasting machine; drying is carried out with vibrated fluidized bed; control EAT 170 degree; leaving air temp 85 degree; carry out screening with square sieve and obtain 20-80 order oxytetracycline calcium granule product 4.9kg, content 20.8% of giving money as a gift, moisture content 3.6%.
Embodiment 2
Measure 60l Performance in Oxytetracycline Fermentation Broth, detection fermentation unit is 33653u/ml, adds calcium carbonate 1.6kg in Performance in Oxytetracycline Fermentation Broth, stirs 5h, carries out calcify reaction; In terramycin calcifying solution, add 1N hcl acidifying, regulate calcifying solution pH to 4.5; Acidifying liquid is pumped into autoclave diaphragm plate-frame filtering, pressure 1Mpa, squeeze to moisture content 50%, obtain oxytetracycline calcium wet cake; Pulverized by oxytetracycline calcium wet cake wet stock pulverizer, granularity is 0.1mm, makes it dispersed; Oxytetracycline calcium wet powder is passed into rotary squeezing granulator (particle diameter 0.8mm) screen cloth to granulate; whole grain 30min is carried out with shot-blasting machine; drying is carried out with vibrated fluidized bed; control EAT 175 degree; leaving air temp 90 degree; carry out screening with square sieve and obtain 10-100 order oxytetracycline calcium granule product 9.7kg, content 19.8% of giving money as a gift, moisture content 2.4%.。
Embodiment 3
Measure 30l Performance in Oxytetracycline Fermentation Broth, detection fermentation unit is 33579u/ml, adds calcium carbonate 0.7kg in Performance in Oxytetracycline Fermentation Broth, stirs 1h, carries out calcify reaction; In terramycin calcifying solution, add 1N hcl acidifying, regulate calcifying solution pH to 6.5; Acidifying liquid is pumped into autoclave diaphragm plate-frame filtering, pressure 1.2Mpa, squeeze to moisture content 42.7%, obtain oxytetracycline calcium wet cake; Pulverized by oxytetracycline calcium wet cake wet stock pulverizer, granularity is 0.6mm, makes it dispersed; Oxytetracycline calcium wet powder is passed into oscillating granulator (particle diameter 0.6mm) screen cloth to granulate; whole grain 60min is carried out with shot-blasting machine; drying is carried out with fluidizing fluid-bed; control EAT 170 degree; leaving air temp 85 degree; carry out screening by spin vibration sieve and obtain 20-80 order oxytetracycline calcium granule product 4.8kg, content 22.4% of giving money as a gift, moisture content 3.8%.
Embodiment 4
Measure 60l Performance in Oxytetracycline Fermentation Broth, detection fermentation unit is 34178u/ml, adds calcium carbonate 1.8kg in Performance in Oxytetracycline Fermentation Broth, stirs 5h, carries out calcify reaction; In terramycin calcifying solution, add 1N hcl acidifying, regulate calcifying solution pH to 4.5; Acidifying liquid is pumped into autoclave diaphragm plate-frame filtering, pressure 1.5Mpa, squeeze to moisture content 44.7%, obtain oxytetracycline calcium wet cake; Pulverized by oxytetracycline calcium wet cake wet stock pulverizer, granularity is 0.2mm, makes it dispersed; Oxytetracycline calcium wet powder is passed into oscillating granulator (particle diameter 1.2mm) screen cloth to granulate; whole grain 30min is carried out with shot-blasting machine; drying is carried out with fluidizing fluid-bed; control EAT 175 degree; leaving air temp 90 degree; carry out screening by spin vibration sieve and obtain 10-100 order oxytetracycline calcium granule product 9.8kg, content 19.3% of giving money as a gift, moisture content 2.7%.
Embodiment 5
Measure 1000l Performance in Oxytetracycline Fermentation Broth, detection fermentation unit is 35278u/ml, adds calcium carbonate 28.2kg in Performance in Oxytetracycline Fermentation Broth, stirs 2h, carries out calcify reaction; In terramycin calcifying solution, add 1N hcl acidifying, regulate calcifying solution pH to 5.5; Acidifying liquid is pumped into autoclave diaphragm plate-frame filtering, pressure 1.4Mpa, squeeze to moisture content 40%, obtain oxytetracycline calcium wet cake; Pulverized by oxytetracycline calcium wet cake wet stock pulverizer, granularity is 1mm, makes it dispersed; Oxytetracycline calcium wet powder is passed into rotary squeezing granulator (0.6mm) screen cloth to granulate; whole grain 30min is carried out with shot-blasting machine; drying is carried out with vibrated fluidized bed; control EAT 200 degree; leaving air temp 100 degree; carry out screening with square sieve and obtain 10-100 order oxytetracycline calcium granule product 169.5kg, content 20.6% of giving money as a gift, moisture content 1.9%.
Embodiment 6
Inventor detects embodiment 1-5 products obtained therefrom according to veterinary drug national standard " veterinary drug provincial standard rising national standard " second (The Ministry of Agriculture of the People's Republic of China, MOA's in September, 2006), and concrete outcome is in table 1.
Table 1
| Detect sample | Content (%) | Moisture (%) | Heavy metal (ppm) | Arsenic (ppm) |
| Embodiment 1 | 20.8 | 3.6 | ≤10 | ≤5 |
| Embodiment 2 | 19.8 | 2.4 | ≤10 | ≤5 |
| Embodiment 3 | 22.4 | 3.8 | ≤10 | ≤5 |
| Embodiment 4 | 19.3 | 2.7 | ≤10 | ≤5 |
| Embodiment 5 | 20.6 | 1.9 | ≤10 | ≤5 |
As can be seen from the data in table 1, the quality of full fermentation oxytetracycline calcium particle of the present invention meets the requirement of quality standard, constant product quality.
Claims (10)
1. a preparation method for full fermentation oxytetracycline calcium particle, is characterized in that, comprise the following steps:
A. in Performance in Oxytetracycline Fermentation Broth, add calcium carbonate, stir, reaction 1-5h, obtains the calcifying solution of terramycin;
Add hydrochloric acid in the calcifying solution of the terramycin b. obtained to step a, the pH value regulating calcifying solution is 4.5-6.5, obtains acidifying solution;
C. the acidifying solution that step b obtains is pumped into autoclave diaphragm sheet frame to filter, the moisture squeezed to filter cake is 40-50%, obtains the filter cake of oxytetracycline calcium;
The filter cake wet stock pulverizer of the oxytetracycline calcium d. obtained by step c is pulverized, and obtains oxytetracycline calcium wet-milling;
E. oxytetracycline calcium wet-milling steps d obtained directly is granulated, whole grain, drying, screening, namely obtain the particle of oxytetracycline calcium.
2. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, is characterized in that, the addition of calcium carbonate described in step a is 0.7-0.9 times of contained terramycin amount in Performance in Oxytetracycline Fermentation Broth.
3. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, is characterized in that, the addition of calcium carbonate described in step a is 0.75-0.8 times of contained terramycin amount in Performance in Oxytetracycline Fermentation Broth.
4. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, it is characterized in that, the time of reacting described in step a is 2h.
5. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, it is characterized in that, the concentration of hydrochloric acid described in step b is 1N.
6. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, is characterized in that, regulate the pH value of calcifying solution to be 5.0-5.5 described in step b.
7. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, it is characterized in that, during the plate-frame filtering of autoclave diaphragm described in step c, squeeze pressure is 1-1.5Mpa.
8. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, it is characterized in that, the moisture of filter cake described in step c is 45%.
9. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, is characterized in that, carry out the grinding particle size≤1mm pulverized described in steps d with wet stock pulverizer.
10. the preparation method of a kind of full fermentation oxytetracycline calcium particle according to claim 1, is characterized in that, the particle diameter of directly granulating described in step e is 0.6-1.2mm, and described screening sieve number is 10-100 order.
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Cited By (7)
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| CN104621360A (en) * | 2015-03-11 | 2015-05-20 | 河北圣雪大成制药有限责任公司 | Preparation method of bacitracin zinc premix |
| CN106721083A (en) * | 2016-12-21 | 2017-05-31 | 驻马店华中正大有限公司 | A kind of terramycin pre-mixing agent and preparation method thereof |
| CN107574218A (en) * | 2017-09-28 | 2018-01-12 | 金河生物科技股份有限公司 | A kind of method of streptomyces rimosus fermenting and producing oxytetracycline calcium pre-mixing agent |
| CN107739746A (en) * | 2017-09-28 | 2018-02-27 | 金河生物科技股份有限公司 | A kind of preparation method and product of oxytetracycline calcium pre-mixing agent for animals |
| CN108029864A (en) * | 2017-10-24 | 2018-05-15 | 浙江汇能生物股份有限公司 | A kind of preparation method of full fermentation terramycin calcium powder |
| CN108058283A (en) * | 2017-12-14 | 2018-05-22 | 烟台只楚化学新材料股份有限公司 | A kind of polyolefin transparent nucleater particle and preparation method thereof of high-purity, high fluidity |
| CN108432949A (en) * | 2018-03-13 | 2018-08-24 | 河北圣雪大成制药有限责任公司 | A kind of production equipment and preparation method of energy-saving and environment-friendly oxytetracycline calcium |
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| CN104621360A (en) * | 2015-03-11 | 2015-05-20 | 河北圣雪大成制药有限责任公司 | Preparation method of bacitracin zinc premix |
| CN106721083A (en) * | 2016-12-21 | 2017-05-31 | 驻马店华中正大有限公司 | A kind of terramycin pre-mixing agent and preparation method thereof |
| CN107574218A (en) * | 2017-09-28 | 2018-01-12 | 金河生物科技股份有限公司 | A kind of method of streptomyces rimosus fermenting and producing oxytetracycline calcium pre-mixing agent |
| CN107739746A (en) * | 2017-09-28 | 2018-02-27 | 金河生物科技股份有限公司 | A kind of preparation method and product of oxytetracycline calcium pre-mixing agent for animals |
| CN108029864A (en) * | 2017-10-24 | 2018-05-15 | 浙江汇能生物股份有限公司 | A kind of preparation method of full fermentation terramycin calcium powder |
| CN108058283A (en) * | 2017-12-14 | 2018-05-22 | 烟台只楚化学新材料股份有限公司 | A kind of polyolefin transparent nucleater particle and preparation method thereof of high-purity, high fluidity |
| CN108432949A (en) * | 2018-03-13 | 2018-08-24 | 河北圣雪大成制药有限责任公司 | A kind of production equipment and preparation method of energy-saving and environment-friendly oxytetracycline calcium |
| CN108432949B (en) * | 2018-03-13 | 2021-06-18 | 河北圣雪大成制药有限责任公司 | Energy-saving and environment-friendly oxytetracycline calcium production equipment and preparation method |
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