CN104872402A - Method for preparing coated ferrous sulfate by using acetylate cross-link starch - Google Patents
Method for preparing coated ferrous sulfate by using acetylate cross-link starch Download PDFInfo
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Abstract
The invention discloses a method for preparing coated ferrous sulfate by using acetylate cross-link starch. The method comprises the following steps: step 100: preparing the acetylate cross-link starch; step 200: melting the acetylate cross-link starch obtained in the step 100, and obtaining the acetylate cross-link starch in a molten state; step 300: adding ferrous sulfate into the acetylate cross-link starch in the molten state and emulsifying, so as to obtain an emulsified mixture; step 400: after sufficient emulsification of the emulsified mixture obtained in the step 300, carrying out high pressure atomizing so as to obtain the coated ferrous sulfate; step 500: carrying out condensation to the coated ferrous sulfate obtained in the step 400. The coated ferrous sulfate prepared through the method provided by the invention is less susceptible to oxidation, excellent in self stability, does not impact vitamins in feed when being combined with other trace elements, adopts a gelatin substitution for coating, and is safe and environment-friendly.
Description
Technical field
The present invention relates to feed additive technology, specifically refer to a kind of preparation method of acetylation crosslinked starch coated ferrous sulphate.
Background technology
Anhydrous slufuric acid ferrous iron is white powder, and containing the crystallization water is pale green crystals, and crystal is commonly called as " green vitriol ", and the water-soluble aqueous solution is light green color.The most often use its glaucous hydrate.At present, in feed, addition manner is mainly and directly adds ferrous sulfate, and this mode mainly exists 2 weak points: one is that ferrous sulfate self stability is poor, in feed formulation process, easily by other oxides in the oxygen in air or feed, cause ferrous sulfate content loss; Two is the stability affecting vitamin.Directly adding ferrous sulfate in feed, during with other trace element (as copper sulphate) compatibility, as supported one's family, very large destruction being have to other composition in feed, extend the residual quantity constantly reducing vitamin in feed with feed Store time.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of acetylation crosslinked starch coated ferrous sulphate; the coated ferrous sulphate obtained by preparation method of the present invention is not oxidizable, self stability good; with the vitamin that can not affect during other micro-compatibility in feed, carry out bag quilt, safety and environmental protection with gelatine replacement.
A preparation method for acetylation crosslinked starch coated ferrous sulphate, comprises the following steps:
Step S100: preparation acetylation crosslinked starch;
Step S200: the acetylation crosslinked starch obtained in melting step S100, obtains the acetylation crosslinked starch of molten condition;
Step S300: add ferrous sulfate and emulsification in the acetylation crosslinked starch of the molten condition obtained in step S200, obtains emulsifying mixt;
Step S400: after the emulsifying mixt obtained in step S300 is fully emulsified, carries out high-pressure fog and obtains coated ferrous sulphate;
Step S500: condensation is carried out to the coated ferrous sulphate obtained in step S400.
Further, described step S100 specifically refers to following steps:
Step S11: the starch size of preparation 30-50%;
The sodium chloride solution of step S12:20-30g/kg and the sodium hydroxide solution of 5-10g/kg add in the starch size described in step S11 simultaneously, and fully stir;
Step S13: the starch size obtained in regulating step S12 is to 30-50 DEG C;
Step S14: the sodium trimetaphosphate solution adding 400-600mg/kg in the starch size described in step S13;
Step S15: after reaction 4-6h, be 8-9 with the starch size obtained in sulfuric acid neutralization procedure S14 to its pH value, the acetic acid of instillation 50-70g/kg, and fully stir;
Step S16: after reaction 0.5-2h, be 5-6 with the starch size obtained in sulfuric acid neutralization procedure S15 to its pH value;
Step S17: the starch size obtained in step S16 is entered successively main centrifuge washing 10-30min, enters concentrated centrifuge washing 30-60min, enters ten two-stage cyclone separator countercurrent washing 30-60min under 40 DEG C of conditions;
Step S18: the starch size obtained in step S17 is sent into the dry 2-4h of evaporator, obtain acetylation crosslinked starch.
First prepare acetylation crosslinked starch in the present invention, then bag quilt is carried out to ferrous sulfate.Described acetylation crosslinked starch, as gelatine replacement, not only has gelatin at bag by the advantage in technique, and compensate for the shortcoming of gelatin, healthy and safe.
Described gelatin is a kind of hydrophilic colloid of the protein generally used, and is by slaughtered animals refuse (as skin, bone), obtained by insoluble collagen being hydrolyzed into solvable gelatin.Collagen is the principal structural component of white tissues fiber, and be present in animal institute in a organized way with in organ, about form 30% of total protein content.Because the numerous characteristics that gelatin has is better than other hydrophilic colloid for food industry, become the thing of the ideal of food processing.But, use gelatin on the pan because of its animal origin recently in the food industry.Traditionally, vegetarianism consumer and the instruction of its religious belief will avoid the consumer coming from animal product (as gelatin) to avoid enjoying the food containing gelatin always.These avoid the consumer enjoying gelatin traditionally, and general satisfaction contains the product of more secondary binding agent in buying, with the selection of the vegetarianism and/or religion that adapt to them.
On the other hand, the ordinary consumer of constraint is not selected because worry that the appearance of prion disease (as rabid ox disease) may be relevant with the gelatin of protein by vegetarianism or religion, also in change thought.Although most of government has taken proper measure and has alleviated the worry of the public to rabid ox disease in Western society, such as, by strictly prohibitting the use by the animal product made with prion disease animal in the food industry, but the public still exists for the worry of the gelatin using protein derived, and seems to increase.Use the acetylation crosslinked starch of nonprotein as gelatine replacement, remain a kind of hydrophilic colloid, not only there is gelatin at bag by the advantage in technique, and compensate for the shortcoming of gelatin, safety and Health.
The present invention has following remarkable result: one is that technique is simple, easy to operate, with low cost; Two is coated ferrous sulphate product with stable quality, not easily be oxidized by the oxygen in air, improve the residual quantity of ferrous sulfate in feed; Three is reduce ferrous sulfate to the destruction of vitamin in feed.
Further, described step S100 specifically comprises the following steps:
Described step S11: the starch size of preparation 40%;
The sodium chloride solution of described step S12:25g/kg and the sodium hydroxide solution of 7.5g/kg add in the described starch size described in step S11 simultaneously, and fully stir;
Described step S13: the starch size to 40 DEG C obtained in regulating step S12;
Described step S14: the sodium trimetaphosphate solution adding 500mg/kg in the starch size described in step S13;
Described step S15: after reaction 5h, with the starch size obtained in sulfuric acid neutralization procedure S14 to PH=8.5, the acetic acid of instillation 60g/kg, and fully stir;
Described step S16: after reaction 0.5h, with the starch size obtained in sulfuric acid neutralization procedure S15 to PH=5.5;
Described step S17: the starch size obtained in step S16 is entered successively main centrifuge washing 20min, enters concentrated centrifuge washing 40min, enters ten two-stage cyclone separator countercurrent washing 50min under 40 DEG C of conditions;
Step S18: the starch size obtained in step S17 is sent into the dry 3h of evaporator, obtain acetylation crosslinked starch.
Further, described step S200 specifically refers to and introduces in smelting furnace by the acetylation crosslinked starch obtained in step S100, regulates temperature of smelting furnace to 70-90 DEG C, stirs 1-3h.
Further, described step S200 specifically refers to and introduces in smelting furnace by the acetylation crosslinked starch obtained in step S100, regulates temperature of smelting furnace to 78-82 DEG C, stirs 2h.
Further, described step S300 specifically refers to following steps:
Step S31: the acetylation crosslinked starch obtained in step S100 is introduced emulsifier, connects emulsifier;
Step S32: carry out first stage emulsification, regulates the rotating speed of emulsifier to 2000rpm-3000rpm, emulsification 20min-30min;
Step S33: add ferrous sulfate;
Step S34: carry out second stage emulsification, regulates the rotating speed of emulsifier to 4000rpm-5000rpm, obtains emulsifying mixt after emulsification 5min-10min.
Further, described step S300 specifically refers to following steps:
Described step S31: the acetylation crosslinked starch after the acetylation crosslinked starch obtained in step S100 is introduced emulsifier, emulsification joint being inserted molten condition, opens emulsifier;
Described step S32: carry out first stage emulsification, regulates the rotating speed of emulsifier to 2500rpm, emulsification 25min;
Described step S33: add ferrous sulfate;
Described step S34: carry out second stage emulsification, regulates the rotating speed of emulsifier to 4500rpm, obtains emulsifying mixt after emulsification 8min.
Further, described step S400 specifically refers to following steps:
Described step S41: emulsifying mixt is moved to high-pressure fog container;
Described step S42: connect air compressor;
Described step S43: spray emulsifying mixt to temperature in the cold air of 0-8 DEG C, obtain coated ferrous sulphate.
Further, described step S43 specifically points to temperature in the cold air of 0-5 DEG C and sprays emulsifying mixt, obtains coated ferrous sulphate.
Further, described step S500 specifically refers to and is positioned in the condensation bin of 0-10 DEG C by coated ferrous sulphate.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) present invention process is simple, easy to operate, with low cost.
(2) coated ferrous sulphate that obtains of the present invention, stay in grade, not easily be oxidized by the oxygen in air, improve the residual quantity of ferrous sulfate in feed.
(3) coated ferrous sulphate that obtains of the present invention, reduces ferrous sulfate to the destruction of vitamin in feed.
(4) use acetylation crosslinked starch as gelatine replacement in the present invention, not only there is gelatin at bag by the advantage in technique, and compensate for the shortcoming of gelatin, healthy and safe.
Accompanying drawing explanation
Fig. 1 is the flow chart of key step of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
The preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate of the present embodiment, as shown in Figure 1, is mainly achieved through the following technical solutions: comprise the following steps:
Step S100: preparation acetylation crosslinked starch;
Step S200: the acetylation crosslinked starch obtained in melting step S100, obtains the acetylation crosslinked starch of molten condition;
Step S300: add ferrous sulfate and emulsification in the acetylation crosslinked starch of the molten condition obtained in step S200, obtains emulsifying mixt;
Step S400: after the emulsifying mixt obtained in step S300 is fully emulsified, carries out high-pressure fog and obtains coated ferrous sulphate;
Step S500: condensation is carried out to the coated ferrous sulphate obtained in step S400.
First prepare acetylation crosslinked starch in the present invention, then bag quilt is carried out to ferrous sulfate.Described acetylation crosslinked starch, as gelatine replacement, not only has gelatin at bag by the advantage in technique, and compensate for the shortcoming of gelatin, healthy and safe.
Embodiment 2:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S100 specifically comprises the following steps:
Described step S11: the starch size of preparation 40%;
The sodium chloride solution of described step S12:25g/kg and the sodium hydroxide solution of 7.5g/kg add in the described starch size described in step S11 simultaneously, and fully stir;
Described step S13: the starch size to 40 DEG C obtained in regulating step S12;
Described step S14: the sodium trimetaphosphate solution adding 500mg/kg in the starch size described in step S13;
Described step S15: after reaction 5h, with the starch size obtained in sulfuric acid neutralization procedure S14 to PH=8.5, the acetic acid of instillation 60g/kg, and fully stir;
Described step S16: after reaction 0.5h, with the starch size obtained in sulfuric acid neutralization procedure S15 to PH=5.5;
Described step S17: the starch size obtained in step S16 is entered successively main centrifuge washing 20min, enters concentrated centrifuge washing 40min, enters ten two-stage cyclone separator countercurrent washing 50min under 40 DEG C of conditions;
Step S18: the starch size obtained in step S17 is sent into the dry 3h of evaporator, obtain acetylation crosslinked starch.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 3:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S200 specifically refers to and introduces in smelting furnace by the acetylation crosslinked starch obtained in step S100, regulates temperature of smelting furnace to 70-90 DEG C, stirs 1-3h.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 4:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S200 specifically refers to and introduces in smelting furnace by the acetylation crosslinked starch obtained in step S100, regulates temperature of smelting furnace to 78-82 DEG C, stirs 2h.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 5:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S300 specifically refers to following steps:
Step S31: the acetylation crosslinked starch obtained in step S100 is introduced emulsifier, connects emulsifier;
Step S32: carry out first stage emulsification, regulates the rotating speed of emulsifier to 2000rpm-3000rpm, emulsification 20min-30min;
Step S33: add ferrous sulfate;
Step S34: carry out second stage emulsification, regulates the rotating speed of emulsifier to 4000rpm-5000rpm, obtains emulsifying mixt after emulsification 5min-10min.
Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 6:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S300 specifically refers to following steps:
Described step S31: the acetylation crosslinked starch after the acetylation crosslinked starch obtained in step S100 is introduced emulsifier, emulsification joint being inserted molten condition, opens emulsifier;
Described step S32: carry out first stage emulsification, regulates the rotating speed of emulsifier to 2500rpm, emulsification 25min;
Described step S33: add ferrous sulfate;
Described step S34: carry out second stage emulsification, regulates the rotating speed of emulsifier to 4500rpm, obtains emulsifying mixt after emulsification 8min.
Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 7:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S400 specifically refers to following steps:
Described step S41: emulsifying mixt is moved to high-pressure fog container;
Described step S42: connect air compressor;
Described step S43: spray emulsifying mixt to temperature in the cold air of 0-8 DEG C, obtain coated ferrous sulphate.
Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 8:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S43 specifically points to temperature in the cold air of 0-5 DEG C and sprays emulsifying mixt, obtains coated ferrous sulphate.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
Embodiment 9:
The present embodiment does further optimization on the basis of above-described embodiment, and further, described step S500 specifically refers to and is positioned in the condensation bin of 0-10 DEG C by coated ferrous sulphate.Other parts of the present embodiment are same as the previously described embodiments, therefore repeat no more.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (10)
1., by a preparation method for acetylation crosslinked starch coated ferrous sulphate, it is characterized in that comprising the following steps:
Step S100: preparation acetylation crosslinked starch;
Step S200: the acetylation crosslinked starch obtained in melting step S100, obtains the acetylation crosslinked starch of molten condition;
Step S300: add ferrous sulfate and emulsification in the acetylation crosslinked starch of the molten condition obtained in step S200, obtains emulsifying mixt;
Step S400: after the emulsifying mixt obtained in step S300 is fully emulsified, carries out high-pressure fog and obtains coated ferrous sulphate;
Step S500: condensation is carried out to the coated ferrous sulphate obtained in step S400.
2. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 1, is characterized in that: described step S100 specifically refers to following steps:
Step S11: the starch size of preparation 30-50%;
The sodium chloride solution of step S12:20-30g/kg and the sodium hydroxide solution of 5-10g/kg add in the starch size described in step S11 simultaneously, and fully stir;
Step S13: the starch size obtained in regulating step S12 is to 30-50 DEG C;
Step S14: the sodium trimetaphosphate solution adding 400-600mg/kg in the starch size described in step S13;
Step S15: after reaction 4-6h, be 8-9 with the starch size obtained in sulfuric acid neutralization procedure S14 to its pH value, the acetic acid of instillation 50-70g/kg, and fully stir;
Step S16: after reaction 0.5-2h, be 5-6 with the starch size obtained in sulfuric acid neutralization procedure S15 to its pH value;
Step S17: the starch size obtained in step S16 is entered successively main centrifuge washing 10-30min, enters concentrated centrifuge washing 30-60min, enters ten two-stage cyclone separator countercurrent washing 30-60min under 40 DEG C of conditions;
Step S18: the starch size obtained in step S17 is sent into the dry 2-4h of evaporator, obtain acetylation crosslinked starch.
3. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 2, is characterized in that: described step S100 specifically comprises the following steps:
Described step S11: the starch size of preparation 40%;
The sodium chloride solution of described step S12:25g/kg and the sodium hydroxide solution of 7.5g/kg add in the described starch size described in step S11 simultaneously, and fully stir;
Described step S13: the starch size to 40 DEG C obtained in regulating step S12;
Described step S14: the sodium trimetaphosphate solution adding 500mg/kg in the starch size described in step S13;
Described step S15: after reaction 5h, with the starch size obtained in sulfuric acid neutralization procedure S14 to PH=8.5, the acetic acid of instillation 60g/kg, and fully stir;
Described step S16: after reaction 0.5h, with the starch size obtained in sulfuric acid neutralization procedure S15 to PH=5.5;
Described step S17: the starch size obtained in step S16 is entered successively main centrifuge washing 20min, enters concentrated centrifuge washing 40min, enters ten two-stage cyclone separator countercurrent washing 50min under 40 DEG C of conditions;
Step S18: the starch size obtained in step S17 is sent into the dry 3h of evaporator, obtain acetylation crosslinked starch.
4. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate described in claim 1-3 any one; it is characterized in that: described step S200 specifically refers to and introduces in smelting furnace by the acetylation crosslinked starch obtained in step S100; regulate temperature of smelting furnace to 70-90 DEG C, stir 1-3h.
5. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 4; it is characterized in that: described step S200 specifically refers to and introduces in smelting furnace by the acetylation crosslinked starch obtained in step S100; regulate temperature of smelting furnace to 78-82 DEG C, stir 2h.
6. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 1-3 any one, is characterized in that: described step S300 specifically refers to following steps:
Step S31: the acetylation crosslinked starch obtained in step S100 is introduced emulsifier, connects emulsifier;
Step S32: carry out first stage emulsification, regulates the rotating speed of emulsifier to 2000rpm-3000rpm, emulsification 20min-30min;
Step S33: add ferrous sulfate;
Step S34: carry out second stage emulsification, regulates the rotating speed of emulsifier to 4000rpm-5000rpm, obtains emulsifying mixt after emulsification 5min-10min.
7. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 6, is characterized in that: described step S300 specifically refers to following steps:
Described step S31: the acetylation crosslinked starch after the acetylation crosslinked starch obtained in step S100 is introduced emulsifier, emulsification joint being inserted molten condition, opens emulsifier;
Described step S32: carry out first stage emulsification, regulates the rotating speed of emulsifier to 2500rpm, emulsification 25min;
Described step S33: add ferrous sulfate;
Described step S34: carry out second stage emulsification, regulates the rotating speed of emulsifier to 4500rpm, obtains emulsifying mixt after emulsification 8min.
8. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 1-3 any one, is characterized in that: described step S400 specifically refers to following steps:
Described step S41: emulsifying mixt is moved to high-pressure fog container;
Described step S42: connect air compressor;
Described step S43: spray emulsifying mixt to temperature in the cold air of 0-8 DEG C, obtain coated ferrous sulphate.
9. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 4, is characterized in that: described step S43 specifically points to temperature in the cold air of 0-5 DEG C and sprays emulsifying mixt, obtains coated ferrous sulphate.
10. the preparation method of a kind of acetylation crosslinked starch coated ferrous sulphate according to claim 1-3 any one, is characterized in that: described step S500 specifically refers to and is positioned in the condensation bin of 0-10 DEG C by coated ferrous sulphate.
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