CN104585480A - Envelope calcium chloride and preparation method thereof - Google Patents

Envelope calcium chloride and preparation method thereof Download PDF

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Publication number
CN104585480A
CN104585480A CN201510071649.7A CN201510071649A CN104585480A CN 104585480 A CN104585480 A CN 104585480A CN 201510071649 A CN201510071649 A CN 201510071649A CN 104585480 A CN104585480 A CN 104585480A
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calcium chloride
parts
preparation
coating
calcium
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CN104585480B (en
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李浙烽
陈强
徐二华
许美芳
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KANGDEQUAN FEED CO Ltd HANGZHOU
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KANGDEQUAN FEED CO Ltd HANGZHOU
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Abstract

The invention discloses envelope calcium chloride and a preparation method thereof. The envelope calcium chloride is prepared from the following raw materials in parts by weight: 5-20 parts of hydrogenated palm oil, 5-20 parts of hydrogenated castor oil, 4-30 parts of silicon dioxide, 1-20 parts of fatty acid calcium and 60-85 parts of calcium chloride. The preparation method is characterized in that the envelope calcium chloride which can be taken as a feed additive is obtained by taking the hydrogenated palm oil, the hydrogenated castor oil, silicon dioxide and fatty acid calcium as envelope materials and taking the calcium chloride as a core material through a multiple-time pelletizing and enveloping technology. The envelope calcium chloride can make up the defects that the calcium chloride raw material easily absorbs water, and also can guarantee that calcium chloride safely passes through a rumen to smoothly reach the intestinal tract, so that the biological utilization rate of calcium chloride is greatly increased.

Description

A kind of coating calcium chloride and preparation method thereof
Technical field
The present invention relates to field of feed additive technology, particularly relate to a kind of coating calcium chloride and preparation method thereof.
Background technology
Calcium chloride is inorganic compound, is a kind of salt be made up of chlorine element and calcium constituent, is typical ionic halide.Calcium chloride molecular formula is CaCl 2, relative molecular mass is 110.98, and proterties is white, hard fragment or particle, micro-hardship, odorless.The hygroscopicity of calcium chloride is extremely strong, and to be exposed in air very easily deliquescence, soluble in water, release a large amount of heat, its aqueous solution is alkalescence simultaneously.
Calcium chloride is often applied in dairy cow diet as anion salt additive, there is anion needed for supplementary milk cow, reduce dairy cow diet DCAD (daily ration ionic equilibrium) value, improve the functions such as milk cow body fluid acid-base balance, effectively can increase the concentration of blood Free Calcium, reduce the generation of low blood calcium, reduce the incidence of disease of milk fever, retention of afterbirth and left displaced abomasums, add the output of milk, improve reproductive performance, improve conception rate.
The common calcium chloride very easily moisture absorption, strong to the mechanical erosion of feed, easily cause feed to lump and destroy other nutritional labelings.In addition, if calcium chloride Direct-fed is easily caused milk cow food refusal, have intense stimulus effect to body tissue, can impact ruminal pH value, during rumen bypass, loss is larger.Therefore, common calcium chloride is not suitable for Direct-fed.
The technological means of carrying out reasonable employment to calcium chloride in prior art mainly contains intravenous injection and calcium chloride gel is fed, but, intravenous injection and the requirement of calcium chloride gel feeding method to operating technology higher, efficiency is lower, and stress be larger to milk cow.In addition to the above methods, film-coating technique is also had, namely by selecting dissimilar coated fertilizer to carry out coating to calcium chloride, prevent the calcium chloride moisture absorption from luming as much as possible, reduce calcium chloride to the stimulation of body, make calcium chloride stable when rumen bypass, reach onset after small intestine.
At present, in feed additive field, types of functionality material obtains stable micro-capsule by the form of coating, then mix with feed or the research of Direct-fed more.Such as: application publication number is that the Patent Application Publication of CN103652366A discloses and a kind of stablizes micro-capsule coating Mercaptamine and preparation method thereof, this stable micro-capsule coating Mercaptamine is made primarily of the raw material that quality proportioning is following: Mercaptamine 20 ~ 55 parts, cornstarch 15 ~ 35 parts, sodium carboxymethylcellulose 0.1 ~ 10 part, sodium alginate 1 ~ 10 part, ethyl cellulose 0.1 ~ 10 part, beta-schardinger dextrin-10 ~ 15 parts, Brazil wax 10 ~ 50 parts.The preparation method of this coating is: by mass concentration be 1 ~ 10% sodium carboxymethyl cellulose solution mix with cornstarch, sodium alginate, ethyl cellulose and beta-schardinger dextrin-after, again the Mercaptamine after heating and melting is joined wherein, carry out fluidized bed granulation, carry out dressing at the Brazil wax adding liquid state, obtain finally stable micro-capsule coating Mercaptamine.
But the film-coating technique being directed to calcium chloride is at present also immature, solve the poor effect of moisture absorption problem, be difficult to promote.Therefore, be necessary to probe into a kind of film-coating technique can avoiding the calcium chloride moisture absorption, for feed additive field provides a kind of stable coating calcium chloride.
Summary of the invention
The invention provides a kind of coating calcium chloride and preparation method thereof, the feed caking that this coating calcium chloride can avoid the calcium chloride moisture absorption to cause, reduction animal directly eats the serious stimulation that calcium chloride causes body tissue, for milk cow supplements sufficient calcium ion and chlorion.
A kind of coating calcium chloride, with parts by weight, comprises following raw material: HPO 5 ~ 20 parts; Rilanit special 5 ~ 20 parts; Silica 4 ~ 30 parts; Fatty acid calcium 1 ~ 20 part; 60 ~ 85 parts, calcium chloride.
As preferably, described coating calcium chloride, with parts by weight, comprises following raw material: HPO 5 ~ 10 parts; Rilanit special 5 ~ 10 parts; Silica 4 ~ 10 parts; Fatty acid calcium 5 ~ 10 parts; 60 ~ 80 parts, calcium chloride.
Wherein, described fatty acid calcium is calcium palmitate.As preferably, in calcium palmitate, the mass fraction of palmitic acid is 43 ~ 45%.
Present invention also offers a kind of preparation method of described coating calcium chloride, comprise the following steps:
(1) using saturated calcium chloride water as mother liquor, using silica as material, carry out mist projection granulating, obtain one-level coated granule;
(2) one-level coated granule and rilanit special, fatty acid calcium are mixed, carry out extruder grain, obtain secondary packet membrane granule;
(3) using liquid hydrogenated palm oil as mother liquor, using secondary packet membrane granule as material, carry out second time mist projection granulating, obtain coating calcium chloride.
Silica is dropped in granulation fluid bed, make it be fluidization, more saturated calcium chloride water is atomized, after atomization, by its spraying in fluidised silica surface, and itself and silica are bondd mutually; In the process, calcium chloride enters in silica hole, and drying is fixed in silica hole after removing moisture.As preferably, in step (1), the technological parameter of mist projection granulating is: EAT is 60 ~ 65 DEG C, and leaving air temp is 50 ~ 55 DEG C, and atomizing pressure is 0.18 ~ 0.2Mpa, and peristaltic pump rotating speed is 200r/min.
In step (2), one-level coated granule and rilanit special, fatty acid calcium incorporation time length can affect the Blending Efficiency of Blending of one-level coated granule and rilanit special, fatty acid calcium, and as preferably, the time of described mixing is 5 ~ 15min.
As preferably, secondary packet membrane granule crosses 12 ~ 30 mesh sieves, guarantees that coated granule can not be excessive, and affects the product quality of subsequent packet membrane process and coating calcium chloride.
As preferably, in step (3), the technological parameter of second time mist projection granulating is: EAT is 45 ~ 60 DEG C, and leaving air temp is 35 ~ 45 DEG C, and atomizing pressure is 0.12 ~ 0.18Mpa, and peristaltic pump rotating speed is 100r/min.
After coating calcium chloride crosses 10 ~ 24 mesh sieves, particle size is the most suitable.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention with HPO, rilanit special, silica and fatty acid calcium for packaging material, take calcium chloride as core, the coating calcium chloride that can be used as feed addictive is obtained by multi granulating film-coating technique, this coating calcium chloride not only compensate for the defect of the easy moisture absorption of calcium chloride raw material, and calcium chloride safety cud can also be ensured, smooth arrival enteron aisle, substantially increases the bioavailability of calcium chloride;
(2) coating calcium chloride of the present invention carries out feeding by mixing with feed, not only avoid because of injection and gel feed to animal cause stress, and this coating calcium chloride occupation mode is easy, and application cost is lower;
(3) coating calcium chloride of the present invention is on the one hand by the calcium balance maintaining milk cow of directly replenishing the calcium, and falls the generation of hypocalcemia, on the other hand by providing anion to reduce dairy cow diet ionic equilibrium value, indirectly falls the generation of hypocalcemia and secondary disease thereof;
(4) coating calcium chloride good fluidity of the present invention, security is high, is convenient to the hybrid process of feed.
Detailed description of the invention
Below in conjunction with specific embodiment and comparative example, the present invention is described further, but protection scope of the present invention is not limited in this.
Embodiment 1
A kind of coating calcium chloride, the concrete steps of its preparation method are as follows:
(1) 600g calcium chloride is got soluble in water, prepare calcium chloride saturated aqueous solution, get 100g silica and drop in granulation fluid bed, with calcium chloride saturated aqueous solution for mother liquor is atomized, and sprayed in fluid bed to silica surface by peristaltic pump, carry out mist projection granulating, in mist projection granulating process, EAT is 62 DEG C, leaving air temp is 55 DEG C, atomizing pressure is 0.2Mpa, and peristaltic pump rotating speed is 200r/min, obtains one-level coated granule;
(2) 100g rilanit special and 100g calcium palmitate (mass fraction of palmitic acid is 43%) are added in mixer, heating and melting at 80 DEG C, then add one-level coated granule, mixing 10min; Said mixture is put into the crowded grain machine that 75kW aperture is 1.0mm, extruder grain, after cooling, cross 30 mesh sieves, obtain secondary packet membrane granule;
(3) 100g HPO is put into reactor, at 80 DEG C, heating and melting obtains liquid hydrogenated palm oil, secondary packet membrane granule is poured in dressing fluid bed, be that mother liquor is atomized by liquid hydrogenated palm oil, and sprayed in fluid bed to secondary packet membrane granule surface by peristaltic pump, carry out second time mist projection granulating, in mist projection granulating process, EAT is 60 DEG C, leaving air temp is 45 DEG C, and atomizing pressure is 0.18Mpa, and peristaltic pump rotating speed is 100r/min, after 20 mesh sieves, obtain the coating calcium chloride that calcium chloride mass fraction is 60%.
Embodiment 2
A kind of coating calcium chloride, the concrete steps of its preparation method are as follows:
(1) 750g calcium chloride is got soluble in water, prepare calcium chloride saturated aqueous solution, get 100g silica and drop in granulation fluid bed, with calcium chloride saturated aqueous solution for mother liquor is atomized, and sprayed in fluid bed to silica surface by peristaltic pump, carry out mist projection granulating, in mist projection granulating process, EAT is 65 DEG C, leaving air temp is 53 DEG C, atomizing pressure is 0.2Mpa, and peristaltic pump rotating speed is 200r/min, obtains one-level coated granule;
(2) 50g rilanit special and 50g calcium palmitate (mass fraction of palmitic acid is 45%) are added in mixer, heating and melting at 80 DEG C, then add one-level coated granule, mixing 12min; Said mixture is put into the crowded grain machine that 75kW aperture is 1.2mm, extruder grain, after cooling, cross 30 mesh sieves, obtain secondary packet membrane granule;
(3) 50g HPO is put into reactor, at 80 DEG C, heating and melting obtains liquid hydrogenated palm oil, secondary packet membrane granule is poured in dressing fluid bed, be that mother liquor is atomized by liquid hydrogenated palm oil, and sprayed in fluid bed to secondary packet membrane granule surface by peristaltic pump, carry out second time mist projection granulating, in mist projection granulating process, EAT is 38 DEG C, leaving air temp is 40 DEG C, and atomizing pressure is 0.16Mpa, and peristaltic pump rotating speed is 100r/min, after 16 mesh sieves, obtain the coating calcium chloride that calcium chloride mass fraction is 75%.
Embodiment 3 ~ 6 and comparative example 1 ~ 3
The coating calcium chloride preparation method of embodiment 3 ~ 6 and comparative example 1 ~ 3 is except parameter listed in table 1 is different from embodiment 1, and all the other contents are identical with embodiment 1.
Adopt the preparation method identical with embodiment 1, some parameter only in preparation method is different; Comparative example 1 is also substantially identical with the preparation method of embodiment 1 with comparative example 2, and only the raw material composition and ratio of coating calcium chloride is different, and comparative example 3 adopts different raw material compositions, and specifically as shown in table 1, the not mentioned part of table 1 is identical with embodiment 1.
The coating calcium chloride obtained carries out the mensuration of dissolution rate, and detection method is:
(1) temperature regulating dissolution test system is 37 DEG C, and rotating speed is 100r/min, pours the simulation rumen liquid of artificial preparation into, open machine in stripping rotor, after equitemperature is stable, for subsequent use;
(2) getting 4g coating calcium chloride sample (being accurate to 0.0002), put into the stripping rotor of the dissolution test system that step (1) has been debugged, detecting respectively at carrying out sampling after 1h, 2h, 4h, 8h.Get 10.00mL filtrate pours in 250mL conical flask at every turn, add 50mL water, the 5mL triethanolamine aqueous solution (volume ratio of triethanolamine and water is 1: 2), 2mL sodium hydroxide solution (concentration is 100g/L) and 0.1g calconum indicator and (get calconum 0.1g, add anhydrous sodium sulfate 10g, grinding evenly, to obtain final product) shake up; Be titrated to till solution becomes pure blue with the EDTA-2Na of 0.05mol/L, be titration end-point, calculate and obtain dissolution rate.
The computing formula of dissolution rate is: dissolution rate=(stripping content/initial content) × 100%.
Preparation method's parameter and result as shown in table 1.
Comparative example 4
With application publication number, disclosed in the Patent Application Publication of CN103238730A, coated fertilizer and coating process carry out coating process to calcium chloride.
A kind of coating calcium chloride, the concrete steps of its preparation method are as follows:
Take 300g calcium chloride water-soluble, again 100g hydroxypropyl methylcellulose, 150g shitosan and 100g silica are mixed, and 230 DEG C of high-boilings expand in fluid bed, then calcium chloride water is sprayed on the mixture of hydroxypropyl methylcellulose, shitosan and silica, calcium chloride is embedded in framework material, and carries out 120 DEG C of high temperature dryings; In-5 DEG C of low-temperature settings after high temperature drying, make calcium chloride granules curing molding, then 200g Brazil wax, 100g palm oil grease and 50g polyethylene glycol are dissolved in organic solvent, end spray is carried out in fluidized-bed coating machine, coated fertilizer even application to calcium chloride granules surface, flow velocity 0.1-3L/min, EAT 90 DEG C, time 3h, the product granularity more than 85% finally formed crosses 20 order analysis sieves.Finally, the coating calcium chloride sample that calcium chloride content is 30% is obtained.
The coating calcium chloride that the method obtains exposes 5min in atmosphere the moisture absorption can become liquid, not easily with other feedstuff Homogeneous phase mixing; And the coating calcium chloride that the method obtains can produce large calorimetric while the moisture absorption, destroy other nutriments in feed.And the good fluidity of product of the present invention, the not easily moisture absorption, and other nutriments in feed can not be damaged.

Claims (10)

1. a coating calcium chloride, is characterized in that, with parts by weight, comprises following raw material: HPO 5 ~ 20 parts; Rilanit special 5 ~ 20 parts; Silica 4 ~ 30 parts; Fatty acid calcium 1 ~ 20 part; 60 ~ 85 parts, calcium chloride.
2. coating calcium chloride as claimed in claim 1, is characterized in that, with parts by weight, comprise following raw material: HPO 5 ~ 10 parts; Rilanit special 5 ~ 10 parts; Silica 4 ~ 10 parts; Fatty acid calcium 5 ~ 10 parts; 60 ~ 80 parts, calcium chloride.
3. coating calcium chloride as claimed in claim 1, it is characterized in that, described fatty acid calcium is calcium palmitate.
4. coating calcium chloride as claimed in claim 3, it is characterized in that, in calcium palmitate, the mass fraction of palmitic acid is 43 ~ 45%.
5. a preparation method for coating calcium chloride as described in as arbitrary in Claims 1 to 4, is characterized in that, comprise the following steps:
(1) using saturated calcium chloride water as mother liquor, using silica as material, carry out mist projection granulating, obtain one-level coated granule;
(2) one-level coated granule and liquid hydrogenated castor oil, fatty acid calcium are mixed, carry out extruder grain, obtain secondary packet membrane granule;
(3) using liquid hydrogenated palm oil as mother liquor, using secondary packet membrane granule as material, carry out second time mist projection granulating, obtain coating calcium chloride.
6. preparation method as claimed in claim 5, is characterized in that, in step (1), the technological parameter of mist projection granulating is: EAT is 60 ~ 65 DEG C, leaving air temp is 50 ~ 55 DEG C, and atomizing pressure is 0.18 ~ 0.2Mpa, and peristaltic pump rotating speed is 200r/min.
7. preparation method as claimed in claim 5, it is characterized in that, the time of described mixing is 5 ~ 15min.
8. preparation method as claimed in claim 5, it is characterized in that, secondary packet membrane granule crosses 12 ~ 30 mesh sieves.
9. preparation method as claimed in claim 5, is characterized in that, in step (3), the technological parameter of second time mist projection granulating is: EAT is 45 ~ 60 DEG C, leaving air temp is 35 ~ 45 DEG C, and atomizing pressure is 0.12 ~ 0.18Mpa, and peristaltic pump rotating speed is 100r/min.
10. preparation method as claimed in claim 5, it is characterized in that, coating calcium chloride crosses 10 ~ 24 mesh sieves.
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106071148A (en) * 2016-06-17 2016-11-09 吉林农业大学 A kind of cow in perinatal period anion salt feed additive and preparation method thereof
CN106220293A (en) * 2016-06-28 2016-12-14 宿松县北浴乡斌峰家庭农场 A kind of preparation method that can effectively improve soil and environmental protection low cost Pseudobulbus Bletillae (Rhizoma Bletillae) special fertilizer
CN106431537A (en) * 2016-06-28 2017-02-22 宿松县北浴乡斌峰家庭农场 Preparation method of low-cost fertilizer-effect-retaining fertilizer special for camellia oleifera
CN106431595A (en) * 2016-06-28 2017-02-22 宿松县北浴乡斌峰家庭农场 Method for preparing special low-cost fertilizer for green tea
CN106721055A (en) * 2016-11-30 2017-05-31 杭州康德权饲料有限公司 Feeding coating compound acidulant and preparation method thereof
CN110200153A (en) * 2019-07-09 2019-09-06 宁夏大田新天地生物工程有限公司 The additive and its application method of the feed supplement of Angus beef essence are raised for preparing paddy
CN110663824A (en) * 2019-10-25 2020-01-10 江苏万瑞达生物科技股份有限公司 Mixed feed for pets and preparation method thereof
CN111011611A (en) * 2019-12-06 2020-04-17 金河生物科技股份有限公司 Micro-capsule calcium chloride for dairy cows and preparation method and application thereof
CN111956604A (en) * 2020-07-10 2020-11-20 福建孚兴药业有限公司 Preparation method of balancing liquid

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CN1925908A (en) * 2003-08-22 2007-03-07 丹尼斯科有限公司 Microcapsules
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106071148A (en) * 2016-06-17 2016-11-09 吉林农业大学 A kind of cow in perinatal period anion salt feed additive and preparation method thereof
CN106220293A (en) * 2016-06-28 2016-12-14 宿松县北浴乡斌峰家庭农场 A kind of preparation method that can effectively improve soil and environmental protection low cost Pseudobulbus Bletillae (Rhizoma Bletillae) special fertilizer
CN106431537A (en) * 2016-06-28 2017-02-22 宿松县北浴乡斌峰家庭农场 Preparation method of low-cost fertilizer-effect-retaining fertilizer special for camellia oleifera
CN106431595A (en) * 2016-06-28 2017-02-22 宿松县北浴乡斌峰家庭农场 Method for preparing special low-cost fertilizer for green tea
CN106721055A (en) * 2016-11-30 2017-05-31 杭州康德权饲料有限公司 Feeding coating compound acidulant and preparation method thereof
CN110200153A (en) * 2019-07-09 2019-09-06 宁夏大田新天地生物工程有限公司 The additive and its application method of the feed supplement of Angus beef essence are raised for preparing paddy
CN110663824A (en) * 2019-10-25 2020-01-10 江苏万瑞达生物科技股份有限公司 Mixed feed for pets and preparation method thereof
CN111011611A (en) * 2019-12-06 2020-04-17 金河生物科技股份有限公司 Micro-capsule calcium chloride for dairy cows and preparation method and application thereof
CN111956604A (en) * 2020-07-10 2020-11-20 福建孚兴药业有限公司 Preparation method of balancing liquid

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