CN104403361B - The technique that a kind of pressurization produces ammonia caramel color - Google Patents
The technique that a kind of pressurization produces ammonia caramel color Download PDFInfo
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- CN104403361B CN104403361B CN201410674605.9A CN201410674605A CN104403361B CN 104403361 B CN104403361 B CN 104403361B CN 201410674605 A CN201410674605 A CN 201410674605A CN 104403361 B CN104403361 B CN 104403361B
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Abstract
The present invention relates to field of food, the technique that a kind of pressurization produces ammonia caramel color.This technique comprises the following steps: 1) feed proportioning: starch sugar is metered into retort, and being assigned to need butt in retort is 60% 90%;2) ammonification: the starch sugar that dispensing is good is cooled to suitable temperature, airtight, in confined conditions, start stirring, start ammonification, control ammonification speed during ammonification thus control pressure inside the tank;3) reaction: in confined conditions, along with the carrying out of ammonification, feed temperature gradually rises, and feed liquid Maillard reaction is carried out therewith, terminates reaction when color rate reaches requirement;4) cooling: after color rate reaches requirement, quickly cooling material is to less than 80 DEG C;5) filter: the material after cooling is filtered, and goes the removal of impurity;6) step such as allotment.The ammonification of this method for once, and is carried out in confined conditions, can more effectively utilize the heat of solution of ammonia, easy to operation.
Description
Technical field
The present invention relates to the production method of burnt sugar coloring in food production, be specially a kind of pressurization and produce ammonia process Jiao
The technique of fried sugar.
Background technology
Burnt sugar coloring is commonly called as caramel, is a kind of one obtained by caramelization or Maillard reaction with glucide
Natural food colour.Burnt sugar coloring is a kind of natural colorant that China allows to use in most food, generally
It is with food stage saccharide such as glucose, fructose, sucrose, Nulomoline, maltose syrup, molasses, Starch Hydrolysis
Sugar waits as raw material, at high temperature (normal pressure or pressurization) be allowed to coking, and process further and prepare.At food
In industry, burnt sugar coloring application is wide, consumption is big.According to coloring agent Professional Committee of China statistics, burnt at present
Fried sugar volume of production and marketing accounts for more than the 90% of whole edible coloring agent.The three meals in a day of almost all people all be unable to do without containing
The food of burnt sugar coloring, so mode of researching and producing is more environmentally friendly, energy consumption consumption is lower, product integrated cost is lower
Burnt sugar coloring production method be a major issue benefited the nation and the people, to caramel industry or even edible coloring agent industry all
There is huge contribution.
Burnt sugar coloring is divided into four big classes according to production method difference, i.e. common law burnt sugar coloring (is commonly called as non-ammonia caramel
Color), ammonia caramel color, sulphite ammonia caramel normal complexion caustic sulfite method burnt sugar coloring.Common law caramel
Color is by with or without acid or alkali, but heats without ammonium or sulfite compound and prepare.Ammonia caramel color
It is in the presence of ammonium compounds, with or without acid or alkali, but does not use sulphite heating to prepare.Sulfurous acid
Ammonium method burnt sugar coloring is in the presence of both sulphite and ammonium compounds, prepares with or without acid or alkali heating.
Caustic sulfite method burnt sugar coloring is in the presence of sulphite, with or without bronsted lowry acids and bases bronsted lowry, but does not use ammonium
Compound heating prepares.Burnt sugar coloring industry mainly uses common law, ammonia process and sulphite burnt sugar coloring technique now
Produce.
The production method of ammonia caramel color, in current industry, most producer uses the non-pressure process mode of production,
The most in atmospheric conditions, with ammonium compounds such as liquefied ammonia, ammonia or ammonium salts as catalyst, it is heated to a constant temperature
Degree, continues to be reacted to terminal.The result that this mode is caused is exactly: one. along with temperature in course of reaction
Rising, part ammonia escapes together with steam, and temperature is the highest, and the amount of effusion is the biggest, and emergent gas contains
Higher ammonia nitrogen and COD, pollute environment.Two. the usage amount of ammonia is relatively big, raises production cost.Three. steam
Consumption is big, and energy consumption is high.
Ye You minority producer uses pressurization to produce ammonia process product recently, but ammonification number of times is frequent, production operation
More complicated, and ammonification inevitable loss partial heat every time, do not have an ammonification convenient for production, energy consumption is the most more
High.
Summary of the invention
The deficiency that the present invention is showed for non-pressure process ammonia caramel color production technology just, and repeatedly ammonification
Pressurization produces the loaded down with trivial details of ammonia caramel color technique, it is provided that the mode of production is easier, more environmentally friendly, energy consumption consumes more
The technique that a kind of pressurization that low, product integrated cost is lower produces ammonia caramel color.
The concrete technical scheme of the present invention is as follows:
A kind of pressurization produces the technique of ammonia caramel color, comprises the following steps:
(1) feed proportioning: starch sugar is metered into retort, is assigned to need butt, typically in retort
It is 60% 90%, finally requires to determine required dispensing butt according to product Baume degrees;With unit mass without
When representing the moisture in wet solid on the basis of water solid, referred to as butt.% herein indicates and accounts for without molasses sugar
The mass percent of sugar liquid.
(2) ammonification: the starch sugar that dispensing is good is cooled to suitable temperature, airtight, in confined conditions, open
Dynamic stirring, starts ammonification, disposably completes ammonification, the good ammonification speed of ammonification process control thus control
Pressure inside the tank.Ammonia residual requires to determine according to product color rate, and high color rate product ammonia residual is relatively big, low color
Rate product ammonia residual is less, or adds the ammonium salts such as corresponding ammonia, ammonium sulfate, ammonium hydrogen carbonate.
(3) reaction: in confined conditions, along with the carrying out of ammonification, because ammonia heat of solution, feed temperature gradually rises
High;Along with the rising feed liquid Maillard reaction of temperature is carried out therewith.And at the beginning of burnt sugar coloring Maillard reaction
Phase can release substantial amounts of heat, and id reaction liberated heat can maintain this reaction to need substantially
Temperature and pressure.Therefore pressurization production ammonia caramel color steam economy in course of reaction is few.
Reaction is terminated when color rate reaches requirement.
(4) cooling: after color rate reaches requirement, quickly cooling material is to less than 80 DEG C.
(5) filter: the material after cooling is filtered, and goes the removal of impurity.
(6) allotment: material is pumped into blend tank, requires to allocate according to the technology of color rate, Baume.
(7) metering filling: deployed product, metering filling, warehouse-in keeping.
Ammonification process described in step (2) is to carry out in confined conditions.For the ease of ammonification, during ammonification
Feed temperature controls 50-90 DEG C;Ammonification speed determines according to reaction pressure inside the tank, 2-10kg the most per minute.
Ammonification process for disposably required ammonia amount is all added, time needed for ammonification a length of 1-5 hour.
Course of reaction described in step (3) is to carry out under an increased pressure, and compressive reaction process maintains reaction
System temperature is 90-150 DEG C;Pressure inside the tank 0.05-0.5Mpa is reacted during reaction;Product color rate reaches requirement
Rear termination reacts.
Cooling procedure described in step (4) in order to reach the purpose quickly cooled down, can use coil pipe cooling and
The modes such as interlayer cool down.
The present invention use ammonification pressurization produce ammonia caramel color, because ammonification, reaction are all close
Carry out under the conditions of closing, do not have gas effusion, so not resulting in ammonia loss, so the amount ratio normal pressure of ammonia
Method is few, effective rate of utilization is higher, thus reduces catalyst cost, it is to avoid pollute environment.And airtight condition
The heat of solution of ammonia, Maillard reaction institute liberated heat can be made full use of, thus be substantially reduced steam consumption,
Save energy consumption, overall reduction product integrated cost.
Compressive reaction temperature is lower.Non-pressure process is because continuous heating, and reaction latter temperature can be up to 180 DEG C,
Pressurization reaction relies on self-heat generation to maintain temperature, reaction gentleness, and temperature has only to 90-150 DEG C, pressurization
Course of reaction is not required to continuous heating, and steam consumes few, and course of reaction does not have gas effusion.So pressurization
Production ammonia caramel color technique production method is more environmentally friendly, energy consumption consumption is lower, product integrated cost is lower.
Therefore pressurization production ammonia caramel color technique can effectively reduce cost, improve product competitiveness in the market;
It is to meet country to reduce energy consumption, energy-saving and emission-reduction principles and policies and comply with a kind of production method in epoch;It is a kind of right
Country, industry, enterprise can bring personal production technology favourable.
The positive effect of the present invention is embodied in:
(1), pressurization produces ammonia caramel color and relatively reduces catalyst with conventional atmospheric method production ammonia caramel color ratio
Consumption, the utilization rate of ammonia is higher.Conventional atmospheric method produces ammonia caramel color owing to being to carry out at ambient pressure,
Along with the raised portion ammonia of reaction temperature escapes together with steam, and pressurization produces ammonia caramel color work
The ammonia that skill adds will not escape, and the burnt sugar coloring product ammonia residual producing mutually homochromy rate can reduce by 10%
15%.The utilization rate of ammonia is higher, reduces catalyst cost simultaneously.
(2) ammonification of this method is for once, and carries out in confined conditions, can more effectively utilize the molten of ammonia
Antipyretic, easy to operation.
(3) the pressurization production ammonification of ammonia caramel color, course of reaction is carried out under an increased pressure, and temperature is than often
Platen press is low, and reaction condition is gentleer, does not have gas and escapes, and favourable improvement working condition will not
Pollutant atmosphere.Meet modern industry production requirement.
(4) pressurization produces ammonia caramel color and produces ammonia caramel color ratio relatively with conventional atmospheric method, and steam consumption quantity is more
Few, reduce production cost.
(5) this technique simplifies, optimizes production technology;Improve product quality;Reduce production cost;Change
It is apt to working condition;Protect environment.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with being embodied as
The present invention is described in further detail for mode, but this should not be interpreted as the scope of the above-mentioned theme of the present invention
It is only limitted to following embodiment.
Embodiment 1:
Produce 36Be, 30000EBC ammonia caramel color.
Estimation: the dispensing butt needed according to caramel product Baume estimation raw material.In view of caramel polycondensation process
In can produce part water, feed proportioning butt is estimated appropriate 75%.
Batching: by 6000kg DE value 97%, butt is the starch sugar syrup metering entrance retort of 70%, opens
Open stirring, heat up and concentrate.Sugar liquid temperature is risen to 115 DEG C by 31 DEG C, sampling detection sugar liquid butt
Content is 75%.Pass vapour cooling, cools down 48 minutes, and sugar liquid temperature is down to 72 DEG C.
Ammonification: confined reaction tank, stirring, ammonia is directly added in sugar liquid, ammonia residual adds by the 3% of raw materials quality,
I.e. needing to add liquefied ammonia 180kg, ammonification speed is 2.6kg/ minute, ammonification duration 70 minutes.Reaction
In tank, temperature is slowly risen to 88 DEG C by 72 DEG C, and pressure inside the tank is gradually increased to 0.175Mpa.Ammonification is complete
Become, disconnect ammonification and connect, close ammonification tube valve.
Compressive reaction: after ammonification completes, confined reaction tank, allow reaction system be in pressurized state, start to open
Opening steam to heat up, otherwise temperature, pressure rises the most wayward.In retort, temperature slowly rises
To 101 DEG C, pressure increases to 0.22Mpa, if temperature can not naturally rise to this temperature and can open stingy.
Then temperature, pressure level-off no longer raise, and maintain this temperature, stress reaction to terminal.Temperature
Timing after degree pressure stability, compressive reaction duration 4 hours 58 minutes.Color rate 0.116 (30526EBC)
Time cooling, terminate reaction.
Cooling: open cooling system, quickly feed liquid is cooled to less than 60 DEG C.
Filter: after cooling, material is filtered, and removes impurity that may be present.
Allotment: material is pumped into blend tank, according to technology requirements such as color rate, Baumes, allocates.Final products
Index is shown in Table one.
(table one)
Metering filling: deployed product, requires metering filling, warehouse-in keeping according to company.
Embodiment 2:
Produce 33Be, 40000EBC ammonia caramel color.
Estimation: the dispensing butt needed according to caramel product Baume estimation raw material.In view of caramel polycondensation process
In can produce part water, feed proportioning butt is estimated appropriate 74%.
Batching: be 98% by 6000kg DE value, butt be 68% starch sugar syrup metering enter retort,
Open stirring, heat up and concentrate.Sugar liquid temperature is risen to 113 DEG C by 29 DEG C, and sampling detection sugar liquid is done
Base is 74%.Pass vapour cooling, cools down 45 minutes, and sugar liquid temperature is down to 70 DEG C.
Ammonification: confined reaction tank, stirring, ammonia is directly added in sugar liquid, ammonia residual adds by the 5% of raw materials quality,
I.e. needing to add liquefied ammonia 420kg, ammonification speed is 3.0kg/ minute, ammonification duration 140 minutes.Instead
In answering tank, temperature is slowly risen to 94 DEG C by 70 DEG C, and pressure inside the tank is gradually increased to 0.205Mpa.Ammonification
Complete, disconnect ammonification and connect, close ammonification tube valve.
Compressive reaction: after ammonification completes, confined reaction tank, allow reaction system be in pressurized state, start to open
Opening steam to heat up, otherwise temperature, pressure rises the most wayward.In retort, temperature slowly rises
To 104 DEG C, pressure increases to 0.285Mpa, if temperature can not naturally rise to this temperature and can open little
Gas.Then temperature, pressure level-off no longer raise, and maintain this temperature, stress reaction to terminal.
Temperature, pressure stably rear timing, compressive reaction duration 5 hours 22 minutes.Color rate 0.153
(40263EBC) cool down time, terminate reaction.
Cooling: open cooling system, quickly feed liquid is cooled to less than 60 DEG C.
Filter: after cooling, material is filtered, and removes impurity that may be present.
Allotment: material is pumped into blend tank, according to technology requirements such as color rate, Baumes, allocates.Final products
Index is shown in Table two.
Metering filling: deployed product, by company's requirement metering filling, warehouse-in keeping.
(table two)
Embodiment 3:
In order to verify that whether pressurization more saves the consumption of ammonia than non-pressure process, still to produce 36Be, 30000EBC ammonia
As a example by method burnt sugar coloring, simply ammonification, reaction are carried out the most at ambient pressure.
Batching: by 6000kg DE value 97%, butt is the starch sugar syrup metering entrance retort of 70%, because of
For being design synthesis under normal pressure, so need not concentrate, the addition of more convenient ammonia.
Ammonification: open stirring, be directly added in sugar liquid by ammonia, ammonia residual, by 3% addition of raw materials quality, i.e. needs
Adding liquefied ammonia 180kg, ammonification speed is 3.0kg/ minute, ammonification duration 60 minutes.Temperature in retort
Degree is slowly risen to 50 DEG C by 39 DEG C, and ammonification completes, and disconnects ammonification and connects, closes ammonification tube valve.
During ammonification, hence it is evident that have ammonia taste to escape in tank, illustrate that ammonia has loss more or less.
Synthesis under normal pressure: after ammonification completes, directly heat up synthesis under normal pressure, reaction duration 6 hours 35 minutes, color rate 0.165
Shi Jiashui terminates reaction.Course of reaction needs persistently material is heated, maintain entering of reaction
OK, material the most very thickness in reaction later stage tank, temperature of charge reaches 155 DEG C.
Cooling: open cooling system, quickly feed liquid is cooled to less than 60 DEG C.
Filter: after cooling, material is filtered, and removes impurity that may be present.
Allotment: material is pumped into blend tank, according to technology requirements such as color rate, Baumes, allocates.Final products
Index is shown in Table three.
(table three)
Be can be seen that by table one, table three, it is bright that non-pressure process produces the burnt sugar coloring product 4 Methylimidazole. content obtained
Aobvious higher than pressurization, even above GB.Illustrate that this Product Safety reduces.Additionally, respectively by embodiment 1,
The burnt sugar coloring product of 3 does Salt tolerance with 20% saline, after standing 24 lab scales, embodiment 1 product without precipitation,
10mm tan precipitate thing is had at the bottom of embodiment 3 product bottle.The reason of appearance precipitation is that the dosage of ammonia is inadequate, says
Bright pressurization more saves the consumption of ammonia than non-pressure process, can effectively reduce catalyst cost, and Product Safety
Higher.
Embodiment 4:
In order to temperature when one of central factor verifying the method reacts is different, more preferable work can or can not be obtained
Skill, still to produce 36Be, 30000EBC ammonia caramel color as a example by, do following single factor experiment.
Temperature when controlling reaction respectively is 95 DEG C, 105 DEG C, 115 DEG C.
Dispensing, ammonification, filter, cool down, allocate same embodiment 1, by external heat or cooling during reaction
Control temperature during reaction.Course of reaction contrasts such as following table four:
(table four)
Reaction temperature | Reaction pressure | Reaction duration | Product color rate | Salt tolerance |
95℃ | 0.175Mpa | 11h45min | 0.115 | 0mm |
105℃ | 0.23Mpa | 4h39min | 0.115 | 0mm |
115℃ | 0.35Mpa | 2h28min | 0.116 | 5mm |
Other index all conformance with standard of product.
As can be seen from Table IV: temperature is the lowest, reaction is too slow, and inefficiency is not suitable for industrialized production;
Temperature is the highest, although can improve efficiency, but product salt tolerance is bad;Considering, reaction temperature is at 100 DEG C
105 DEG C appropriate.
Embodiment 5:
Have a clear superiority in verify that the present invention compares with repeatedly ammonification pressing technology, still to produce 36Be,
As a example by 30000EBC ammonia caramel color, simply ammonification becomes three ammonifications.
Batching: be 98% by 6000kg DE value, butt be 68% starch sugar syrup metering enter retort,
Open stirring, heat up and concentrate.Sugar liquid temperature is risen to 115 DEG C by 30 DEG C, and sampling detection sugar liquid is done
Base is 75%.
Ammonification is reacted: confined reaction tank, opens stirring, is directly added in sugar liquid by ammonia, and ammonia residual presses raw material
1% addition of quality, i.e. needs to add liquefied ammonia 60kg, and ammonification speed is 2.2kg/ minute, ammonification duration
27 minutes.Open retort jacket steam simultaneously.In retort, temperature is slowly risen to by 115 DEG C
124 DEG C, pressure inside the tank is gradually increased to 0.22Mpa.Ammonification completes, and disconnects ammonification and connects, continues
Continuous temperature reaction, every 10 minutes sampling detection color rates.After 30 minutes, color rate is 0.036, reaction
Temperature 131 DEG C in tank, pressure 0.285Mpa.
Secondary ammonification is reacted: after an ammonification is reacted 30 minutes, reacts pressure inside the tank 0.285Mpa, temperature 131 DEG C.
Carry out secondary ammonification, if now directly ammonification due in tank temperature, pressure higher, ammonia is difficult to add,
Or pressure inside the tank drastically raises, processing safety declines, and requires to strengthen to tank body and tank material,
Unfavorable commercial production, it is therefore desirable to first pressure inside the tank is laid down part.Open pressure relief valve, by tank
Interior pressure unloads to 0.200Mpa, then be slowly added into raw materials quality 1% liquefied ammonia amount, i.e. need liquid feeding
Ammonia 60kg, ammonification speed is 1.2kg/ minute, ammonification duration 50 minutes.In retort temperature by
130 DEG C slowly rise to 136 DEG C, and pressure inside the tank is gradually increased to 0.305Mpa.Insulation reaction, every
10 minutes sampling detection color rates.After 30 minutes, color rate is 0.082, temperature 139 DEG C in retort,
Pressure 0.325Mpa.
Three ammonifications are reacted: after secondary ammonification is reacted 30 minutes, react pressure inside the tank 0.325Mpa, temperature 139 DEG C.
Carry out three ammonifications, if now directly ammonification can run into the problem as secondary ammonification, and now
Temperature, pressure is the most highly difficult bigger, it is therefore desirable to first pressure inside the tank is laid down part.Open pressure-relief valve
Door, unloads pressure inside the tank to 0.200Mpa, and temperature is cooled to 130 DEG C, then be slowly added into former
The liquefied ammonia amount of material quality 1%, i.e. needs to add liquefied ammonia 60kg, and ammonification speed is 1.0kg/ minute, ammonification
Duration 60 minutes.In retort, temperature is slowly risen to 138 DEG C by 130 DEG C, and pressure inside the tank is gradually
Rise to 0.310Mpa.Three ammonifications sample detection immediately after completing, now color rate has been 0.117
(30789EBC), reaction is terminated immediately.
Cooling below, filter, allocate same embodiment 1.Final products index is shown in Table five.
(table five)
By embodiment 1 and embodiment 5 it can be seen that repeatedly ammonification compare with an ammonification, repeatedly ammonification operation
Process is complicated, and wayward, and product index and an ammonification product index are close, steam consumption quantity ratio one
Secondary ammonification is big.Therefore the present invention compares with repeatedly ammonification pressurization more apparent advantage.
Steam saving calculates:
If steam saving is described as a example by producing 6 tons of starch sugar butts, 4.0 ten thousand EBC ammonia process products.Produce 6
Ton starch sugar butt, 4.0 ten thousand EBC ammonia process product needed add liquefied ammonia about 420kg, and the heat of solution of ammonia is
34748J/mol, so it is 8.65 × 10 that 420kg liquefied ammonia add feed liquid can produce heat5Kilojoule.One ton of steam
Heat be 3.165 × 106Kilojoule, so the heat that 420kg liquefied ammonia produces is equivalent to 272kg steam and produces
Heat.If employing synthesis under normal pressure, calculate the heat taken away because of moisture evaporation, it is assumed that raw material is initial dry
Base is 75%, and it is 95% that synthesis under normal pressure terminates butt, then the moisture needing volatilization is 6000kg ÷ 75%-6000
÷ 95% ≈ 1684kg;And the heat evaporating one ton of water needs is 2.1 × 106Kilojoule heat, so evaporation
1684kg water needs 3.536 × 106Kilojoule heat, equivalent steam is 1117kg.Therefore pressurization is used to produce
Ammonia caramel normal complexion non-pressure process produces ammonia caramel color ratio product more per ton can save steam about (1117+272)
÷7≈198kg.If calculating by annual 20000 tons of ammonia process products of production and can saving steam 3960 tons, simultaneously
Reduce this link of environmental protection treatment, be substantially reduced production cost.Meet country and reduce energy consumption, energy-saving and emission-reduction
Principles and policies, are favorably improved the competitiveness of product in market.
Claims (2)
1. the technique that a pressurization produces ammonia caramel color, it is characterised in that comprise the following steps:
(1) feed proportioning: starch sugar is metered into retort, being assigned to need butt in retort is 60%-90%;
(2) ammonification: the starch sugar that dispensing is good is cooled to suitable temperature, in confined conditions, starts stirring, starts ammonification, control ammonification speed thus control pressure inside the tank during ammonification;Described ammonification process is to carry out in confined conditions, and for the ease of ammonification, during ammonification, feed temperature controls 100-105 DEG C;Ammonification speed determines according to reaction pressure inside the tank, for 2-10kg per minute, described ammonification process for disposably required ammonia amount is all added, time needed for ammonification a length of 1-5 hour;
(3) reaction: in confined conditions, along with the carrying out of ammonification, feed temperature gradually rises, and feed liquid Maillard reaction is carried out therewith, terminates reaction when color rate reaches requirement;Described course of reaction is to carry out under an increased pressure, and compressive reaction process maintains temperature of reaction system to be 90-150 DEG C;Pressure inside the tank 0.05-0.5MPa is reacted during reaction;Product color rate terminates reaction after reaching requirement;
(4) cooling: after color rate reaches requirement, quickly cooling material is to less than 80 DEG C;
(5) filter: the material after cooling is filtered, and goes the removal of impurity;
(6) allotment: material is pumped into blend tank, requires to allocate according to the technology of color rate, Baume;
(7) metering filling: deployed product, metering filling, warehouse-in keeping.
The technique that pressurization the most according to claim 1 produces ammonia caramel color, it is characterised in that: the cooling procedure described in step (4), in order to reach the purpose quickly cooled down, uses coil pipe cooling and sandwich like way to cool down.
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