CN104231664A - Production method of water-soluble lac red pigment - Google Patents
Production method of water-soluble lac red pigment Download PDFInfo
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- CN104231664A CN104231664A CN201410444491.9A CN201410444491A CN104231664A CN 104231664 A CN104231664 A CN 104231664A CN 201410444491 A CN201410444491 A CN 201410444491A CN 104231664 A CN104231664 A CN 104231664A
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Abstract
The invention relates to a production method of water-soluble lac red pigment, belonging to the technical field of a food additive and solving the problems that the lac red pigment is difficultly soluble into water and bad for application in the food additive. The production method comprises the following steps sequentially: placing lac red pigment into a sodium bicarbonate water liquid, stirring and dissolving, to obtain a lac red water liquid; filtering the lac red water liquid through an ultrafiltration membrane to obtain ultrafiltrate; leading the ultrafiltrate to pass through cationic resin to obtain an extracting liquid; performing vacuum concentration to the extracting liquid to obtain a concentrated liquid; transferring the concentrated liquid into a cold-hot cylinder and heating to 65DEG C, then adding sucrose fatty acid ester for stirring until entire dissolving is achieved, then adding into a homogenous emulsifying machine for emulsifying, to obtain an emulsion; heating the emulsion to 85 DEG C for performing sterilization, to obtain a liquid product; and performing spray-drying to the liquid product by adopting a spray dryer to obtain the water-soluble lac red pigment powder. By adopting the method, the water-soluble lac red pigment easily dissolving into water can be prepared.
Description
Technical field
The invention belongs to technical field of food additives, particularly a kind of modification processing method of Lac dye.
Background technology
Lac dye is through extraction, refining and obtain from the resinous substance lac secreted by the female worm of the tachardia lacca parasitized pulse family, moraceae plants (Laccifer lacca).Solvability: be insoluble in water (0.0335g/20g, 20 DEG C), be slightly soluble in 95% ethanol (0.916g/20g), be soluble in sodium bicarbonate, sodium carbonate and sodium hydroxide solution.
Because Lac dye is insoluble in water, significantly limit its operation strategies.
Summary of the invention
Be insoluble in water for solving Lac dye, be unfavorable for the problem applied in food, the invention provides a kind of production method of water-soluble Lac dye, its technical scheme is as follows:
A production method for water-soluble Lac dye, comprises following sequential steps:
Step 1: dissolve:
Get Lac dye and put into sodium bicarbonate aqueous solution, after stirring and dissolving, leave standstill 2 hours, obtain the red aqueous solution of lac;
Wherein the solvent of sodium bicarbonate aqueous solution is water, and in sodium bicarbonate aqueous solution, the weight percent concentration of sodium bicarbonate is 0.6%;
The weight ratio of Lac dye and sodium bicarbonate aqueous solution is 1:200 ~ 240;
Step 2: ultrafiltration membrance filter:
Red for lac aqueous solution ultra-filtration membrane is filtered, obtains ultrafiltrated;
Step 3: resin absorption:
Ultrafiltrated is passed through resin cation (R.C.) with the flow velocity of 250 ls/h, from the outlet conduit of resin cation (R.C.), obtains extracting solution;
Step 4: concentrated:
Being adopted by extracting solution concentration tank to carry out vacuumizing, to be concentrated into proportion be 1.10 kilograms per cubic meter, obtains concentrated solution;
When wherein vacuumizing concentrated, vacuum degree control is in-0.04 ~-0.08 megapascal (MPa), and controlling thickening temperature is 60 DEG C;
Step 5: emulsification:
Get the hot water that sucrose fatty ester puts into 80 DEG C to dissolve, obtain emulsifying agent;
Wherein the weight ratio of sucrose fatty ester and Lac dye is 5:1000, and the weight ratio of sucrose fatty ester and hot water is 1:2;
Concentrated solution is moved in Cooling or heating jar after being heated to 65 DEG C, add emulsifying agent and carry out being stirred to whole dissolving, obtain emulsifying material;
Then emulsifying material is dropped in homogeneous emulsifying machine and carry out emulsification, obtain emulsion;
Step 6: sterilization:
After emulsion being heated to 85 DEG C, keeping carrying out sterilising treatment in 20 ~ 30 minutes, obtain liquiform product;
Step 7: spraying dry:
Adopt spray-drier to carry out spraying dry to liquiform product, obtain water-soluble Lac dye powder.
Preferably, in described step 2, the aperture of ultra-filtration membrane is 0.002 ~ 0.1 micron, and molecular weight cut-off is 500 ~ 500000, and the working pressure of ultra-filtration membrane both sides is 0.07 ~ 0.7 megapascal (MPa).
Preferably, in described step 3, the weightmeasurement ratio of Lac dye and resin cation (R.C.) is 1:5.
Preferably, in described step 7, the rotating speed controlling the spraying disc in spray-drier is 18000 revs/min, and the inlet temperature controlling spray-drier is 200 ~ 210 DEG C, and temperature out is 70 ~ 75 DEG C.
The object of the inventive method is under the prerequisite not changing the original composition of Lac dye, the Lac dye being insoluble in water is processed into water-soluble Lac dye completely soluble in water, and the solubleness of the water-soluble Lac dye prepared by the inventive method under the temperature condition of 20 DEG C in water reaches more than 10g/100g.
The inventive method is realized by following steps: with common Lac dye for raw material
dissolve with sodium bicarbonate aqueous solution
through ultrafiltration membrance filter
resin cation (R.C.) is refined
vacuum concentration
emulsification
sterilization
spraying dry
packaging, obtains pulverulent water-soluble Lac dye.
The inventive method does not change the composition of Lac dye, can not introduce impurity yet.By test of many times and production practice, water-soluble Lac dye yield prepared by the inventive method is more than 80%, and look valency reaches as high as 150, absorbancy >=0.75, and soluble in water, the indexs such as absorbancy, PH, lead, arsenic meet GB4571-1996 " foodstuff additive Lac dye ".
embodiment
The producer of the equipment used in following embodiment, model and working parameter are as follows:
Ultra-filtration membrane: Shijiazhuang Fei Yue Environmental Protection Technology Co., Ltd produces, model 25-12, and the aperture of film is 0.002 ~ 0.1 μm, and molecular weight cut-off is 500 ~ 500000, and its working pressure is at 0.07-0.7MPa;
Resin cation (R.C.): Langfang City Zhong Huanshuisuo Chemical Co., Ltd. produces, and model is 001x7<732#>;
Concentration tank: State-run Changshu Pharmaceutical Machinery Factory produces, model: ZN100, and vacuum degree control is-0.04 to-0.08MPa;
Cooling or heating jar: Zhejiang Wenxiong Machine Valve Co., Ltd produces, model: LRG-200-00;
Homogeneous emulsifying machine: Hefei calf light industry and machinery company limited produces, model: 2.2;
Spray-drier: Xishan city, Jiangsu Province spray-drier factory produces, model: QZR-25.
Below in conjunction with embodiment, the present invention is illustrated further.
The present invention be a kind of solubleness in pure water is only 0.1% Lac dye, be retrofit into the method for water-soluble Lac dye completely soluble in water.
Embodiment 1:
(1) dissolve: the sodium bicarbonate aqueous solution being 0.6% by the weight percent concentration of 10kg Lac dye 2000kg carries out stirring and dissolving, leave standstill 2 hours, obtain the red aqueous solution of lac;
(2) membrane filtration: red for lac aqueous solution ultra-filtration membrane is carried out pressure filtration at normal temperatures, obtains ultrafiltrated;
(3) resin cation (R.C.) process: allow ultrafiltrated with the flow velocity of 250 L/h by 50L resin cation (R.C.), impurity absorption is on resin, and pigment then flows out with water, from the outlet conduit of resin cation (R.C.), obtain extracting solution; For ensureing that impurity is fully by resin absorption, the envelope-bulk to weight ratio of resin and Lac dye controls at 5:1, and the envelope-bulk to weight ratio of resin and ultrafiltrated is 1:40;
(4) concentrated: to adopt concentration tank to vacuumize extracting solution concentrated, vacuum degree control ,-0.04 to-0.08MPa, concentrates control temperature 60 DEG C, and the quantity obtaining concentrated solution is 33kg, and this concentrated solution is 1.15 at the proportion of 25 DEG C;
(5) emulsification: the hot water dissolving's sucrose fatty ester 50g first using 80 DEG C of 100 g, obtains emulsifying agent 150 grams; Then concentrated solution being moved in Cooling or heating jar and be heated to 65 DEG C, adding emulsifier for mixing to all dissolving; Then carry out emulsification with homogeneous emulsifying machine, the working speed of mulser is 2880 revs/min, obtains emulsion;
(6) sterilization: after being slowly heated to 85 DEG C to emulsion, keeps carrying out sterilising treatment in 20 to 30 minutes, obtains liquiform product;
(7) spraying dry: adopt spray-drier spraying dry is carried out to liquiform product, control in spray-drying process spraying disc rotating speed 18000 revs/min, inlet temperature 200 ~ 210 DEG C, temperature out 70 ~ 75 DEG C; Final acquisition water-soluble Lac dye powder 8.3kg.
Through using pure water to carry out solubility test, 10 grams of water-soluble lac rouge and powder ends are dissolved completely in 100 grams of pure water, and look liquid is bright; And the indexs such as absorbancy, PH, lead, arsenic meet GB4571-1996 " foodstuff additive Lac dye ", detected result is in table one.
Embodiment 2:
(1) dissolve: the sodium bicarbonate aqueous solution being 0.6% by the weight percent concentration of 20kg Lac dye 4400kg carries out stirring and dissolving, leave standstill 2 hours, obtain the red aqueous solution of lac;
(2) membrane filtration: red for lac aqueous solution ultra-filtration membrane is carried out pressure filtration at normal temperatures, obtains ultrafiltrated;
(3) resin cation (R.C.) process: allow ultrafiltrated with the flow velocity of 250 L/h by 100L resin cation (R.C.), impurity absorption is on resin, and pigment then flows out with water, from the outlet conduit of resin cation (R.C.), obtain extracting solution; For ensureing that impurity is fully by resin absorption, the envelope-bulk to weight ratio of resin and Lac dye controls at 5:1, and the envelope-bulk to weight ratio of resin and ultrafiltrated is 1:40;
(4) concentrated: to adopt concentration tank to vacuumize extracting solution concentrated, vacuum degree control ,-0.04 to-0.08MPa, concentrates control temperature 60 DEG C, and the quantity obtaining concentrated solution is 65.3kg, and this concentrated solution is 1.15 at the proportion of 25 DEG C;
(5) emulsification: the hot water dissolving's sucrose fatty ester 100g first using 80 DEG C of 200 g, obtains emulsifying agent 300 grams; Then concentrated solution being moved in Cooling or heating jar and be heated to 65 DEG C, adding emulsifier for mixing to all dissolving; Then carry out emulsification with homogeneous emulsifying machine, the working speed of mulser is 2880 revs/min, obtains emulsion;
(6) sterilization: after being slowly heated to 85 DEG C to emulsion, keeps carrying out sterilising treatment in 20 to 30 minutes, obtains liquiform product;
(7) spraying dry: adopt spray-drier spraying dry is carried out to liquiform product, control in spray-drying process spraying disc rotating speed 18000 revs/min, inlet temperature 200 ~ 210 DEG C, temperature out 70 ~ 75 DEG C; Final acquisition water-soluble Lac dye powder 16.5kg.
Through using pure water to carry out solubility test, 10 grams of water-soluble lac rouge and powder ends are dissolved completely in 100 grams of pure water, and look liquid is bright; And the indexs such as absorbancy, PH, lead, arsenic meet GB4571-1996 " foodstuff additive Lac dye ", detected result is in table one.
Embodiment 3:
(1) dissolve: the sodium bicarbonate aqueous solution being 0.6% by the weight percent concentration of 30kg Lac dye 7200kg carries out stirring and dissolving, leave standstill 2 hours, obtain the red aqueous solution of lac;
(2) membrane filtration: red for lac aqueous solution ultra-filtration membrane is carried out pressure filtration at normal temperatures, obtains ultrafiltrated;
(3) resin cation (R.C.) process: allow ultrafiltrated with the flow velocity of 250 L/h by 150L resin cation (R.C.), impurity absorption is on resin, and pigment then flows out with water, from the outlet conduit of resin cation (R.C.), obtain extracting solution; For ensureing that impurity is fully by resin absorption, the envelope-bulk to weight ratio of resin and Lac dye controls at 5:1, and the envelope-bulk to weight ratio of resin and ultrafiltrated is 1:40;
(4) concentrated: to adopt concentration tank to vacuumize extracting solution concentrated, vacuum degree control ,-0.04 to-0.08MPa, concentrates control temperature 60 DEG C, and the quantity obtaining concentrated solution is 98.5kg, and this concentrated solution is 1.15 at the proportion of 25 DEG C;
(5) emulsification: the hot water dissolving's sucrose fatty ester 150 first using 80 DEG C of 300 g, obtains 450 grams of emulsifying agents; Then concentrated solution being moved in Cooling or heating jar and be heated to 65 DEG C, adding emulsifier for mixing to all dissolving; Then carry out emulsification with homogeneous emulsifying machine, the working speed of mulser is 2880 revs/min, obtains emulsion;
(6) sterilization: after being slowly heated to 85 DEG C to emulsion, keeps carrying out sterilising treatment in 20 to 30 minutes, obtains liquiform product;
(7) spraying dry: adopt spray-drier spraying dry is carried out to liquiform product, control in spray-drying process spraying disc rotating speed 18000 revs/min, inlet temperature 200 ~ 210 DEG C, temperature out 70 ~ 75 DEG C; Final acquisition water-soluble Lac dye powder 24.6kg.
Through using pure water to carry out solubility test, 10 grams of water-soluble lac rouge and powder ends are dissolved completely in 100 grams of pure water, and look liquid is bright; And the indexs such as absorbancy, PH, lead, arsenic meet GB4571-1996 " foodstuff additive Lac dye ", detected result is in table one.
After remodeling process, the Lac dye being insoluble in water becomes water colo(u)r soluble in water, and its range of application in food is significantly increased.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
The quality index of water-soluble Lac dye prepared by table one the present invention
| project | gB4571-1996 index | embodiment 1 | embodiment 2 | embodiment 3 |
| absorbancy (E 0.01% 0.5cm, 490nm) | >=0.65 | 0.7584 | 0.7618 | 0.7751 |
| weight loss on drying, % | ≤ 10 | 6.09 | 6.42 | 7.59 |
| pH value | 3.0 ~ 4.0 | 5.00 | 4.99 | 5.14 |
| plumbous (Pb), mg/kg | ≤ 5 | 0.042 | 0.034 | 0.031 |
| arsenic (As), mg/kg | ≤ 2 | 0.007 | 0.009 | 0.030 |
| solvability in pure water | -----* | 10 grams are dissolved in 100 grams of pure water completely, and look liquid is bright. | 10 grams are dissolved in 100 grams of pure water completely, and look liquid is bright. | 10 grams are dissolved in 100 grams of pure water completely, and look liquid is bright. |
* standard does not specify, but in water, solubleness is only 0.0335g/20g(20 DEG C), and look liquid is for being suspended shape, unclarity.
Claims (4)
1. a production method for water-soluble Lac dye, is characterized in that, comprises following sequential steps:
Step 1: dissolve:
Get Lac dye and put into sodium bicarbonate aqueous solution, after stirring and dissolving, leave standstill 2 hours, obtain the red aqueous solution of lac;
Wherein the solvent of sodium bicarbonate aqueous solution is water, and in sodium bicarbonate aqueous solution, the weight percent concentration of sodium bicarbonate is 0.6%;
The weight ratio of Lac dye and sodium bicarbonate aqueous solution is 1:200 ~ 240;
Step 2: ultrafiltration membrance filter:
Red for lac aqueous solution ultra-filtration membrane is filtered, obtains ultrafiltrated;
Step 3: resin absorption:
Ultrafiltrated is passed through resin cation (R.C.) with the flow velocity of 250 ls/h, from the outlet conduit of resin cation (R.C.), obtains extracting solution;
Step 4: concentrated:
Being adopted by extracting solution concentration tank to carry out vacuumizing, to be concentrated into proportion be 1.10 kilograms per cubic meter, obtains concentrated solution;
When wherein vacuumizing concentrated, vacuum degree control is in-0.04 ~-0.08 megapascal (MPa), and controlling thickening temperature is 60 DEG C;
Step 5: emulsification:
Get the hot water that sucrose fatty ester puts into 80 DEG C to dissolve, obtain emulsifying agent;
Wherein the weight ratio of sucrose fatty ester and Lac dye is 5:1000, and the weight ratio of sucrose fatty ester and hot water is 1:2;
Concentrated solution is moved in Cooling or heating jar after being heated to 65 DEG C, add emulsifying agent and carry out being stirred to whole dissolving, obtain emulsifying material;
Then emulsifying material is dropped in homogeneous emulsifying machine and carry out emulsification, obtain emulsion;
Step 6: sterilization:
After emulsion being heated to 85 DEG C, keeping carrying out sterilising treatment in 20 ~ 30 minutes, obtain liquiform product;
Step 7: spraying dry:
Adopt spray-drier to carry out spraying dry to liquiform product, obtain water-soluble Lac dye powder.
2. the production method of a kind of water-soluble Lac dye according to claim 1, is characterized in that:
In described step 2, the aperture of ultra-filtration membrane is 0.002 ~ 0.1 micron, and molecular weight cut-off is 500 ~ 500000, and the working pressure of ultra-filtration membrane both sides is 0.07 ~ 0.7 megapascal (MPa).
3. the production method of a kind of water-soluble Lac dye according to claim 1 and 2, is characterized in that:
In described step 3, the weightmeasurement ratio of Lac dye and resin cation (R.C.) is 1:5.
4. the production method of a kind of water-soluble Lac dye according to claim 3, is characterized in that:
In described step 7, the rotating speed controlling the spraying disc in spray-drier is 18000 revs/min, and the inlet temperature controlling spray-drier is 200 ~ 210 DEG C, and temperature out is 70 ~ 75 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105341749A (en) * | 2015-11-16 | 2016-02-24 | 重庆市盛沿食品有限责任公司 | Pork sausage |
| CN109735132A (en) * | 2019-01-16 | 2019-05-10 | 云南通海杨氏天然产物有限公司 | The preparation method of cape jasmine purpurin |
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