CN104861736A - Preparation method of caramel pigment without 4-methylimidazole - Google Patents
Preparation method of caramel pigment without 4-methylimidazole Download PDFInfo
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- CN104861736A CN104861736A CN201510218233.3A CN201510218233A CN104861736A CN 104861736 A CN104861736 A CN 104861736A CN 201510218233 A CN201510218233 A CN 201510218233A CN 104861736 A CN104861736 A CN 104861736A
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- methylimidazole
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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Abstract
The invention discloses a preparation method of a caramel pigment without 4-methylimidazole. The preparation method comprises the following steps of: 1) sugar-melting, to be specific, adding a sugar source to a reaction kettle with a condensing and draining device while mixing, turning on a heating device for heating, melting the sugar source after the temperature of the reaction kettle rises above the melting point of the sugar source; 2) draining, to be specific, turning on condensing water, collecting cooling water, and controlling the volume of the cooling water to 5%-8% of the volume of the sugar source; 3) caramelization reaction, to be specific, after draining is finished, changing a condenser pipe into a cooling water return pipe, and keeping at 150 DEG C to 170 DEG C for 1 h-2 h; 4) diluting (neutralizing), to be specific, before the caramelization reaction is finished, adding an alkaline solution to the reaction system slowly to adjust the pH value of the system to be close to the isoelectric point of the caramel pigment, and mixing slowly and continuously until complete reaction is finished; 5) obtaining the product, to be specific, obtaining liquid caramel pigment without 4-methylimidazole after the reaction. The preparation method of the caramel pigment without 4-methylimidazole is economical, practical, safe and high in quality, industrial production is realized, and quality of the caramel pigment is controlled.
Description
Technical field
The invention belongs to foodstuff additive field, be specifically related to a kind of preparation method without 4-methylimidazole caramel colorant.
Background technology
Caramel colorant, have another name called dark reddish brown, caramel colour, be that glucide (hydrolysate etc. as maltose, white sugar, molasses, Nulomoline, lactose, malt syrup and starch) at high temperature dewaters, the complicated sorrel of decomposition and aggregation or chocolate mixture, wherein some is colloid aggregate, is to apply more half-natural food colorant.
China adopts ammonia process to produce caramel colorant mostly, in caramelize process, easy production 4-methylimidazole, 4-methylimidazole is white to off-white color crystalline powder, water-soluble and ethanol, be corrosive, be the by product of ammonia caramel pigment production process, it can cause animal bearing tumor, likely brings carcinogenic risk to human body, although there is no direct evidence, cause some panic thus.
China is flavouring production big country, and caramel colorant is the main additive of seasonings, and its safety in production is to guaranteeing that human health is extremely important.Ammonia caramel pigmentary colour rate is higher, but haematochrome index is lower, to add the seasonings cook vegetables of caramel colorant, vegetables Yi Fawu.
China's caramel colorant production history is long, and before the nineties in last century, mostly adopt workshop-based production, raw materials for production are mainly sweet potato waste, and corn cerealose, glucose mother liquid, ammoniacal liquor, ammonium sulfate etc., mainly pursue high look rate this period.After the nineties so far, reactor is applied in the production of caramel colorant, and industrialization degree improves, quality product significantly improves, and the raw material of production has glucose mother liquid, molasses etc., while requiring yield, propose the concept of haematochrome, yellow pigment index, give the intension that caramel colorant is new.Look rate and red (Huang) pigment indices are the concepts of conflict, and generally speaking, the caramel colorant that look rate is high, red (Huang) pigment indices is lower.The caramel colorant that red (Huang) pigment indices is high, the vegetable colour making soy sauce culinary art being raw material with it is bright-coloured, tempting.
In order to obtain the caramel colorant of Gao Hong (Huang) pigment indices, as far as possible adopting the raw material that purity is high, as glucose, white sugar, but burning due to the personnel of causing easy to foaming in caramelize process, therefore little suitability for industrialized production.From the documents and materials delivered, take glucose as main raw material, add amine substance, as ammonium sulfate, ammonium chloride, ammoniacal liquor, urea, monosodium glutamate etc., prepared the caramel colorant of high haematochrome index in the case of a high temperature, in essence, this reaction belongs to ammonia caramel pigment.And be raw material with white sugar, the method document producing caramel colorant only has introduction, and Hangzhou food factory adopts Shaanxi Tech Univ's technology to adopt manual decoction method to produce, and quality product is better, but cannot large-scale promotion produce.
Summary of the invention
It is raw material with white sugar that object of the present invention provides a kind of, and product is without 4-methylimidazole, high haematochrome, security, high-quality caramel colorant preparation method.As the soy sauce of raw material production, the vegetables of culinary art are bright in colour, not easy oxidation discoloration.
The present invention is achieved through the following technical solutions:
Without a preparation method for 4-methylimidazole caramel colorant, comprise the following steps:
1) molten sugar: add sugared source while stirring in the reactor of band condensate drain device, open heating devices heat, the temperature of question response still rises to more than the fusing point in sugared source, and sugared source starts fusing;
2) draining: open water of condensation, collect water coolant, cooling water inflow should control for sugared source measure 5% ~ 8%;
3) caramelization: after draining terminates, changes into prolong and cools back water pipe, at 150 DEG C ~ 170 DEG C, keep 1h ~ 2h;
4) (neutralization) is diluted: before caramelization terminates, to the iso-electric point of pH value close to caramel colorant slowly adding alkaline solution regulation system in reaction system, be constantly stirred to slowly and react completely;
5) product: after above-mentioned reaction, obtains not containing the aqueous caramel colorant of 4-methylimidazole.
As a further improvement on the present invention, the speed of described stirring is 20-30r/min.
As a further improvement on the present invention, in caramelization step, when foam is more, quickening stirring velocity is 40-60r/min.
As a further improvement on the present invention, described alkali is the Na of 4%-10%
2cO
3the aqueous solution, its add-on is the 45%-50% of sugared source quality.
As a further improvement on the present invention, described pH is 4.5 ~ 6.5.
As a further improvement on the present invention, described sugared source is sucrose, is selected from rock sugar, white sugar, cotton white sugar or brown sugar (Saccharum Sinensis Roxb.).
As a further improvement on the present invention, in described molten sugared step, the temperature of reactor rises to 185 ~ 190 DEG C.
Compared with prior art, the present invention has following useful technique effect:
Take sucrose as raw material, adopt caramelization to prepare caramel colorant, owing to not adding amine substance in reaction system, (inorganic ammonia, as ammoniacal liquor, volatile salt, ammonium chloride, ammonium sulfate etc.; Organic amine, as Sodium Glutamate, amino acid etc.), therefore not containing 4-methylimidazole in caramel colorant.Adopt condensate drain technology, the moisture in removing system, makes balance carry out to the direction of positive reaction, is conducive to the carrying out of caramelization.Water shoot, after suitably dewatering, is become cooling tube, carries out caramelization at this temperature by system.After caramelization terminates, slowly add in alkaline solution He in caramelization process and produce too much acid, improve salt tolerant, the acid resistance of caramel colorant.At high temperature glycan molecule cracking, form aldehyde compound, aldehyde compound high temperature oxidation forms acid, makes the iso-electric point of pH value close to caramel colorant of system, unstable to salt (acid).The method is a kind of preparation method of economical and practical security high quality caramel colorant; Achieve the suitability for industrialized production of this caramel colorant preparation method, control the quality of caramel colorant; The caramel colour plain color rate of producing is moderate, but red (Huang) pigment indices higher (being greater than 9.1) is that ammonia caramel pigment cannot be reached, the vegetable in order to the soy sauce culinary art of its preparation is bright in colour, placing the nondiscoloration of 15 ~ 30min vegetable, is a kind of high-quality caramel colorant.
Further, adopt speed change to stir and eliminate foaming process, the cracking of caramelization process glycan molecule, produces a large amount of CO
2, forming foam, in order to prevent causing because of foaming caramel colorant to overflow tank (reactor) outward in caramelization, causing damage and burning accident.
Further, the alkali added is sodium carbonate, because sodium carbonate alkalescence is soft, meets the requirement of foodstuff additive.
Embodiment
The present invention includes following steps:
(1) molten sugar
Molten sugar: add sucrose while stirring in the reactor of band condensate drain device, open heating devices heat, when the temperature of question response still rises to 190 DEG C, sucrose starts fusing, all fusings in 5min-10min.
(2) draining:
Open water of condensation, collect water coolant, cooling water inflow should control the 5%-8% of sucrose amount.
(3) caramelization:
After draining terminates, prolong is changed into and cools back water pipe, at 150 DEG C-170 DEG C, keep 1h-2h.Owing to producing CO in caramelization
2, so bubble more severe this time, by changing stirring velocity, reach the object eliminating foam
(4) dilute (neutralization):
Before caramelization terminates, to the Na slowly adding 4%-10% in reaction system
2cO
3the aqueous solution regulates pH to be 4.5 ~ 6.5, and add-on is the 45%-50% of sucrose amount, constantly stirs, anti-Spill stopping pan.
(5) check
According to related standards, the look rate of caramel colorant, red (Huang) pigment indices, salt tolerance, acid resistance, viscosity, charging property, 4-methylimidazole content (confirming whether there is the characteristic peak of 4-methylimidazole in caramel colorant by infrared chromatography) are tested.
Caramel colorant is mixed with the solution of 10%, is heated to boil, bean curd is cut into the bar shaped of rule, puts into caramel colorant liquid, pull out after heating 10min, observe bean curd color and luster, change the changing conditions of color and luster more in time, and compare with commercially available caramel colorant.
This technology take sucrose as raw material, obtains caramel colorant by molten sugar, dehydration, polymerization, and the chromophoric group of this caramel colorant is cyclic conjugated π key or-C=O-C=O-key, owing to not having amino in reaction system, therefore does not form 4-methylimidazole.The key of this technology is: the moisture 1., in time in discharge system.The first step of caramelization is dehydration reaction, discharges moisture in time, is conducive to the carrying out of dehydration reaction, after system dehydration, maintains reaction and carries out in the case of a high temperature (polyreaction need at high temperature be carried out).2., select suitable in and the time, caramelization is an acid-producing, in a heated condition, glycan molecule cracking, forms aldehyde compound to system, aldehyde forms acid through oxidation, too low pH value, makes caramel easily reach iso-electric point, easily precipitates in salt solution, therefore, select suitable in and the time, neutralization pH value to caramel stability, there is certain meaning.3., CO is produced in caramelization
2, therefore reaction process foaming phenomena is serious, control another key that foam is this technology, this test reaches the object of froth breaking by changing stirring velocity.Effectively prevent the loss and operator's scald that cause because of foaming in caramelize process.
Embodiment 1:
Limit is stirred (20r/min) limit and add 100kg white sugar in the reactor of band cooling drainage device, opens heating devices heat, and when the temperature of question response still rises to 190 DEG C, sucrose starts fusing, all fusings in 8min.Open water of condensation, collect 5kg water coolant.After draining terminates, prolong is changed into and cools back water pipe, at 150 DEG C, keep 2h.Owing to producing CO in caramelization
2.So bubble more severe this time, by changing stirring velocity (40r/min), reach the object eliminating foam.Before caramelization terminates, to the Na slowly adding mass concentration 5% in reaction system
2cO
3aqueous solution 50kg regulates pH to be 4.5 ~ 6.5, constantly stirs, anti-Spill stopping pan.Salt tolerant (acid), haematochrome index 9.5 can be obtained, not containing the caramel colorant of 4-methylimidazole.
The caramel colorant obtained is mixed with the solution of concentration 10%, is heated to boil, bean curd is cut into the bar shaped of rule, puts into caramel colorant liquid, pull out after heating 10min, find that bean curd is in golden yellow, glossy, in 30min, color and luster is substantially constant.With certain famous brand soy sauce commercially available for raw material, test according to same step, after finding 20min, bean curd color and luster sends out crow.
Embodiment 2:
Limit is stirred (30r/min) limit and add the cotton white sugar of 100kg in the reactor of band condensate drain device, and open heating devices heat, when the temperature of question response still rises to 190 DEG C, sugar starts fusing, all fusings in 9min.Open water of condensation, collect 6kg water coolant.After draining terminates, prolong is changed into and cools back water pipe, at 160 DEG C, keep 1.5h.Owing to producing CO in caramelization
2.So bubble more severe this time, by changing stirring velocity (60/rmin), reach the object eliminating foam.Before caramelization terminates, to the Na slowly adding concentration 9% in reaction system
2cO
3aqueous solution 50kg regulates pH to be 4.5 ~ 6.5, constantly stirs, anti-Spill stopping pan.Salt tolerant (acid), haematochrome index 9.2 can be obtained, not containing the caramel colorant of 4-methylimidazole.
The caramel colorant obtained is mixed with the solution of concentration 10%, is heated to boil, bean curd is cut into the bar shaped of rule, puts into caramel colorant liquid, pull out after heating 10min, find that bean curd is in golden yellow, glossy, in 30min, color and luster is substantially constant.With certain famous brand soy sauce commercially available for raw material, test according to same step, both discoveries are almost as broad as long.
Embodiment 3:
(20r/min) adds 100kg rock sugar in the reactor of band condensate drain device while stirring, opens heating devices heat, and when the temperature of question response still rises to 190 DEG C, sugar starts fusing, all fusings in 10min.Open water of condensation, collect water coolant 6kg.After draining terminates, prolong is changed into and cools back water pipe, at 170 DEG C, keep 1h.Owing to producing CO in caramelization
2.So bubble more severe this time, by changing stirring velocity (50r/min), reach the object eliminating foam.Before caramelization terminates, to the Na slowly adding concentration 10% in reaction system
2cO
3aqueous solution 45kg regulates pH to be 4.5 ~ 6.5, constantly stirs, anti-Spill stopping pan.Salt tolerant (acid), haematochrome index 9.1 can be obtained, not containing the caramel colorant of 4-methylimidazole.
The caramel colorant obtained is mixed with the solution of concentration 10%, is heated to boil, bean curd is cut into the bar shaped of rule, puts into caramel colorant liquid, pull out after heating 10min, find that bean curd is in golden yellow, glossy, in 30min, color and luster is substantially constant.With certain famous brand soy sauce commercially available for raw material, test according to same step, both discoveries difference is little.
Technology point precaution of the present invention:
1., the first step of caramelization is the dehydration reaction of sugar, adopts band cooling drainage device to remove moisture in reaction system in time, ensures that the direction that reaction generates to caramel colorant is carried out.2., draining to after to a certain degree, change water shoot into condensing reflux pipe in time, reacting balance carried out, prevents carbonization.3. because sugared decarboxylation forms CO in, caramelize process
2, therefore very easily bubble, rapid stirring be adopted, reach the object of mechanical defoaming.4., in caramelization process, sugared cracking forms aldehyde, oxidation of aldehydes formation acid, give caramel colorant flavour on the one hand, on the other hand, reduce the pH value in system, when the iso-electric point of system pH close to caramel colorant, bad stability, caramel colorant not salt tolerant, not acidproof.Finite concentration Na is added in system before adopting caramelize to terminate
2cO
3, make the iso-electric point of pH value away from caramel colorant of system, improve salt tolerant (acid) stability of caramel colorant.
Claims (7)
1. without a preparation method for 4-methylimidazole caramel colorant, it is characterized in that, comprise the following steps:
1) molten sugar: add sugared source while stirring in the reactor of band condensate drain device, open heating devices heat, the temperature of question response still rises to more than the fusing point in sugared source, and sugared source starts fusing;
2) draining: open water of condensation, collect water coolant, cooling water inflow should control for sugared source measure 5% ~ 8%;
3) caramelization: after draining terminates, changes into prolong and cools back water pipe, at 150 DEG C ~ 170 DEG C, keep 1h ~ 2h;
4) dilution neutralization: before caramelization terminates, to the iso-electric point of pH value close to caramel colorant slowly adding alkaline solution regulation system in reaction system, be constantly stirred to slowly and react completely;
5) product: after above-mentioned reaction, obtains not containing the aqueous caramel colorant of 4-methylimidazole.
2. a kind of preparation method without 4-methylimidazole caramel colorant according to claim 1, is characterized in that, the speed of described stirring is 20-30r/min.
3. a kind of preparation method without 4-methylimidazole caramel colorant according to claim 2, is characterized in that, in caramelization step, when foam is more, quickening stirring velocity is 40-60r/min.
4. a kind of preparation method without 4-methylimidazole caramel colorant according to claim 1, is characterized in that, described alkali is the Na of 4%-10%
2cO
3the aqueous solution, its add-on is the 45%-50% of sugared source quality.
5. a kind of preparation method without 4-methylimidazole caramel colorant according to claim 1, is characterized in that, described pH is 4.5 ~ 6.5.
6. a kind of preparation method without 4-methylimidazole caramel colorant according to claim 1, is characterized in that, described sugared source is sucrose.
7. a kind of preparation method without 4-methylimidazole caramel colorant according to claim 6, is characterized in that, in described molten sugared step, the temperature of reactor rises to 185 ~ 190 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062132A (en) * | 2015-09-10 | 2015-11-18 | 千禾味业食品股份有限公司 | Ammonium sulfite method-based caramel colour production process |
| CN105295431A (en) * | 2015-11-11 | 2016-02-03 | 广州甘蔗糖业研究所 | Method for preparing cane sugar-based caramel pigment by ammonia method |
| CN105368090A (en) * | 2015-11-21 | 2016-03-02 | 浙江大学 | Preparation method of caramel pigment with reduced 4-methylimidazole content |
| CN106590022A (en) * | 2016-11-04 | 2017-04-26 | 陕西科技大学 | Method for preparing multipurpose caramel pigments by using ultrafiltration technology |
| CN106590024A (en) * | 2016-11-04 | 2017-04-26 | 陕西科技大学 | Preparation method of caramel pigment |
| CN107011696A (en) * | 2017-05-26 | 2017-08-04 | 陕西科技大学 | A kind of common caramel colorant of salt tolerance and its preparation method and application |
| CN108065175A (en) * | 2017-12-30 | 2018-05-25 | 杨烨天 | A kind of preparation method and its production equipment of low viscosity caramel colorant |
| CN114868956A (en) * | 2022-05-11 | 2022-08-09 | 河北中烟工业有限责任公司 | Tobacco colorant, preparation method thereof and cigarette |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062132A (en) * | 2015-09-10 | 2015-11-18 | 千禾味业食品股份有限公司 | Ammonium sulfite method-based caramel colour production process |
| CN105295431A (en) * | 2015-11-11 | 2016-02-03 | 广州甘蔗糖业研究所 | Method for preparing cane sugar-based caramel pigment by ammonia method |
| CN105295431B (en) * | 2015-11-11 | 2017-03-08 | 广州甘蔗糖业研究所 | A kind of method that non-ammonia method prepares sucrose base caramel color |
| CN105368090A (en) * | 2015-11-21 | 2016-03-02 | 浙江大学 | Preparation method of caramel pigment with reduced 4-methylimidazole content |
| CN106590022A (en) * | 2016-11-04 | 2017-04-26 | 陕西科技大学 | Method for preparing multipurpose caramel pigments by using ultrafiltration technology |
| CN106590024A (en) * | 2016-11-04 | 2017-04-26 | 陕西科技大学 | Preparation method of caramel pigment |
| CN107011696A (en) * | 2017-05-26 | 2017-08-04 | 陕西科技大学 | A kind of common caramel colorant of salt tolerance and its preparation method and application |
| CN107011696B (en) * | 2017-05-26 | 2019-08-27 | 青岛日辰食品股份有限公司 | A kind of common caramel colorant of salt tolerance and its preparation method and application |
| CN108065175A (en) * | 2017-12-30 | 2018-05-25 | 杨烨天 | A kind of preparation method and its production equipment of low viscosity caramel colorant |
| CN114868956A (en) * | 2022-05-11 | 2022-08-09 | 河北中烟工业有限责任公司 | Tobacco colorant, preparation method thereof and cigarette |
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