CN104195271A - Method for producing refined sugar through ion-exchange fiber high efficiency decolorization one-step method - Google Patents
Method for producing refined sugar through ion-exchange fiber high efficiency decolorization one-step method Download PDFInfo
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Abstract
The invention provides a method for preparing refined sugar through an ion-exchange fiber high efficiency decolorization one-step method. The method comprises the following steps: (1) conducting pre-treatment on sugar juice obtained through sugar preparation by a sulfurous acid method and a carbonic acid method; (2) conducting negative-positive-negative three-stage pillar exchange decolorization by adopting ion-exchange fiber until the sugar juice reaches the requirements of a refined sugar clear juice, and collecting into a clear juice box; (3) unloading sugar; (4) evaporating the refined sugar clear juice; (5) boiling sugar; (6) conducting help-crystallization and purging. According to the method provided by the invention, on the basis of the conventional sugar preparation process, the ionic fiber exchange process is added, the two-step method is replaced by the one-step method, and the refined sugar is prepared by directly using the sugar juice obtained through sugar preparation by the sulfurous acid method and the carbonic acid method, so that the technology is simple, the quality index of the sugar juice is improved, the product quality is good, the energy is saved, and the environmental pollution is reduced.
Description
Technical field
The present invention relates to sugaring, the specifically production technology of refined sugar, the more specifically method of ion-exchange fiber efficient decolorizing One-step production refined sugar.
Background technology
Along with the raising day by day of living standards of the people, people have higher requirement to the quality of white sugar, and the technology of refined sugar is progressively developed.Existing refined sugar technique is to use two step method, first makes raw sugar, after raw sugar back dissolving, makes refinery liquor by decolorizing with activated carbon, ion-exchange resin decolorization, recrystallizes into refined sugar.The weak point of this technique needs secondary crystal exactly, and steam consumption increases, and increases energy consumption; Traditional sulfurous method and carbonatation process can only boiling plantation white sugars, and quality can reach high-quality sugar and first sugar standard.
The color and luster of white sugar and colour are one of main indexs of white sugar quality.Sugar juice decoloring is always one of common technology difficult problem of sugar industry, is also a most important process in refined sugar industry, and the existing sugaring cleaning technique of China adopts sulfurous method and carbonatation process mostly.
Sulfurous method is gained the name as purification agent taking lime and sulfurous gas, and the number of the complexity of its manufacture method, equipment flowsheet, processing condition and consumable material is between lime method and carbonatation process, and sulfurous method can produce arable land white sugar.
Carbonatation process is the higher method for manufacturing sugar of a kind of peace and quiet effect, be the sucrose purification method using lime and carbonic acid gas as main detergent, its peace and quiet effect is better than sulfurous method, but filter mud is more difficult, its equipment used is more than sulfurous method, thereby production cost is higher.
Not only complex process of these two kinds of decoloration process, facility investment is high, and sugar recovery is low, and amount of lime consumption is large, and filter mud is seriously polluted; And the easy flavescence of color in finished product storage process, second-rate and unstable.
In sugar products, the kind of pigment is a lot, and composition and the character of various pigments have very big difference.There is the original pigment of sugarcane itself, also have a large amount of newly-generated colored substances in process of production, or the dark matter being generated through chemical action by original colourless or light material; There is aromatic (phenol, Flavonoid substances etc., all have aromatic ring), also have (there is no phenyl ring) of non-aromatic; Have low-molecular-weight, intermediate molecular weight, also have high molecular; Have electronegative, micro-chargedly or uncharged, also have with both sexes electric charge; Some raises their color with pH value and greatly deepens, and also some variation is not very big; Some colored substance is more easily removed by clarifying treatment, and some is difficult to remove.
The research of Bento is pointed out, low-molecular-weight aldehydes matter content in sugarcane juice accounts for 65% of total aldehydes matter, and in sugar beet juice, account for 45%, because in treating process, low-molecular-weight aldehydes matter more easily enters in sucrose crystal, so garden beet syrup can directly make white sugar, and sucrose will just can make white sugar through further decolouring.
In sugar manufacturing process, original multiple light color or colourless low-molecular-weight organic matter in sugar cane juice, can produce various chemical reactions and generate the dark matter of high molecular.These reaction as: the oxidation of aldehydes matter and condensation; Flavonoid is cracked into phenol and quinones substance, they again polycondensation become polymer substance, they are with comprehensively amino acid whose and further react; The coking of sucrose; Reducing sugar and amino acid whose reaction (comprise the reaction of series of complex, be commonly referred to Mei Lade or step and strangle reaction); The decomposition of fructose and the polycondensation of product thereof; Oxygen and iron participate in and have strengthened relevant reaction etc. and all can generate the dark matter of high molecular, and they enter in sucrose crystal with higher ratio than original pigment.Raw sugar is more containing this class colored substance, therefore the colour of its retro-dissolved syrup is very high.
Syrup after clarification decolorizing and refining again, traditional method is to use bone black, it has good decolouring and removes the usefulness of deashing, but the investment cost of equipment (particularly reclaim equiment) is large, and newly-built sugar refinery is seldom used.After 20 century 70s, generally use granulated active carbon and ion exchange resin, more thorough to removing of pigment and ash content, they can be regenerated but cost is higher, and also some sugar refinery is used powdered carbon.
Gac is good at absorption and is removed aromatic series organism, and the pigment in sugar products is mainly polyphenol substance, be well suited for activated carbon decolorizing, but gac can not be removed inorganics, will be combined with ion exchange resin for this reason.
Sulfurous method is current conventional decoloring method.A large amount of research and practices all prove, sulfurous gas can suppress the polycondensation of unsaturated compounds in liquid glucose and white sugar, suppress Maillard reaction, reduce the increase of material colour.Variable color when white sugar is deposited is oxygenizement, and sulfurous gas has reductibility because of it, can weaken oxygenizement, reduces the variable color of white sugar, and these are all abroad generally to admit.Therefore,, although the beet-sugar factory purification effect of Europe and USSR (Union of Soviet Socialist Republics) is very high, also generally uses clear juice sulphur to float with syrup sulphur and float.The weak point that this method in use comes out is in syrup, to have introduced non-sugar, thereby makes the quality of syrup and final sucrose crystal all can the reagent of syrup alkalify is affected because having added, and sulphur can be residual in sucrose crystal.
Hydrogen peroxide (H for Mane J D etc.
2o
2) as the discoloring agent of sucrose slurry, evidence H
2o
2except having direct bleaching effect, also have and significantly reduce the effect that coloring matter generates, so H
2o
2as a kind of auxiliary agent of good production high-quality white sugar, its bleaching effect has caused the attention of sugar industry.
The key of producing refined sugar is can be by the pigment in syrup and Impurity removal.Have a lot of scientific research personnel all studying, attempt to carry out One-step production refined sugar in conjunction with traditional sulfurous method and carbonatation process, and research makes some progress.For example Yunnan Qu Xi sugar refinery just makes spent ion exchange resin carry out the research of this respect, and China's Shunde sugar refinery, overseas Chinese sugar refinery, Guangzhou have utilized raw sugar to use ion-exchange resin decolorization to manufacture refined sugar.
Ion exchange technique plays an important role in modern sugar industry.In sugar manufacturing process, because ion-exchange is at the various impurity of removing in liquid glucose, particularly adsorbs, exchange coloring matter and ash content aspect and demonstrated its excellent performance, can improve purification effect, reduce non-sugar content in molasses.Therefore, process syrup by ion exchange method, not only can improve sucrose quality product, and can increase the recovery of sugar.
Over nearly 20～30 years, ion exchange technique has obtained good application in sugar industry abroad.In recent years the research report that relevant ion exchange method is processed syrup decolorization, desalination increases year by year, adopts ion exchange technique to carry out sucrose precision work to have represented the developing direction of modern sugar-refining industry.
Ion exchange method is as the method that replaces charcoal, bone carbon, absorbent charcoal fine purification syrup, has that column flow rate is large, decolouring scope is wide, decolouring capacity is large, can reuse, and foreign ion is had to the advantage such as ramollescence or deionization.Recently, along with the development of ion exchange technique, resin and dynamical process combination mode thereof that multiple applicable high concentration sucrose solution refining is used are succeeded in developing, substantially can obtain very high decolorizing effect and processing power, greatly improve the quality of syrup, improve the productive rate of commerieal sugar, and be convenient to management, and investment and working cost are all starkly lower than the method for other bone black or gac.Therefore, ion exchange method has become the main technique route of refined sugar industry.
Ion exchange resin has a large amount in variety, and the function of having nothing in common with each other and characteristic can, according to the feature of processing requirement and material, be selected suitable resin and combination thereof.More use macroporous strong basic resin anion(R.A), polystyrene or acrylic acid series in refinery.They are good at adsorbing the pigment in liquid glucose, and particularly electronegative pigment also can adsorb the organism that molecular weight is larger, and loading capacity is larger, the impurity wash-out that can it be adsorbed with sodium chloride solution and regenerating.Acrylic resin anti-pollution, more easily regeneration, before being conventionally placed on; Phenylethylene resin series is good at adsorbing aromatic series organism, comprises the composition that acrylic resin is difficult to remove, and it can use separately, also two kinds of resin series connection can be used.
Although having obtained being widely used in syrup decolorization process, ion exchange resin also there is obvious shortcoming, mainly that ion exchange resin belongs to coarse pored structure, its bleaching principle belongs in hole exchange, and in decolorization, duct is easily stopped up, thereby making to return washes difficulty.Because the absorption exchange velocity of resin is slower, in the sugar refining technology flow process of large flow, the investment of switching equipment will be increased simultaneously.Be exactly that exchange resin regeneration is slower in addition, and waste liquid after regeneration is difficult to reclaim, to environment.So ion-exchange-resin process still can not adapt to the requirement of the clear juice of cane sugar factory well.
Ion-exchange fiber and Ion Exchange Resin Phase ratio, maximum difference be just it be fiber surface exchange instead of hole in exchange, therefore do not exist duct to stop up, return the problem such as difficulty, regeneration difficulty of washing, and absorption exchange velocity ratio is very fast, thereby become a good carrier processing the clear juice of cane sugar factory.
Ion-exchange fiber is a kind of novel ion-exchange material, is applied to the research of sugar industry first appeared in nineteen eighty-three.Toshio Yoshioka and Masaharu Shimamura adopt vinylbenzene fabric of island-in-sea type ion-exchange fiber to carry out the experimental study of sucrose retro-dissolved syrup decolouring, have proved that ion-exchange fiber has the decolorization rate and the decolorizing efficiency that are better than resin for syrup decolorization.Consider that ion-exchange fiber specific surface area is large, the material (as pigment) that molecular weight is larger is easily in fiber surface and duct diffusion, adopt ion-exchange fiber directly to process cane sugar, refine out refined sugar by likely realizing on the basis of improving existing sugar refining technology, thereby there is important practical significance.
Professor Huang Yuegang of Guangxi University uses VS-2 type ion-exchange fiber to be studied sub-method sugarcane subsider juice decolouring decalcification, its result of study shows: average purity improves 1.62%, average percent of decolourization 68.86%, average decalcification rate 52.07%, has fully shown that ion-exchange fiber is at the due good prospect in sub-method sugar refinery.
Science and Technology Inst. of Liaoyuan City is used Domestic V S-2 type ion-exchange fiber to process sugar beet molasses in Fan Jiatun sugar refinery, and average percent of decolourization is 79%, and purity improves 1.6%, and average decalcification rate is 48.6%, and after decolouring, syrup thermostability and resistance of oxidation are strong.
Topaz south is waited and installed treatment capacity in Zhong Shan sugar refinery is the pilot plant unit of 20 tons of syrup every day, and in sugar refinery is produced, operation continuously, processes the raw sugar syrup 60～650BX through the floating heat-clearing method of secondary, approximately 75 DEG C.Approximately bimestrial data show continuously, liquid glucose colour 150～170IU after processing, and percent of decolourization is average 75.8%, undoubtedly can boiling refined sugar by this syrup colour.The regeneration period of decolouring fibre columns is 12 hours, with 5% salt water reuse, and 2～3 hours time.Result of study shows the effective of this method, more easily carries out, and has good development prospect.Early stage, the use VS-2 of each seminar type ion-exchange fiber was PVA series, be taking polyvinyl alcohol fiber (PVA) as matrix, by grafting after dehydration carbonization, introduce quaternary amine base, change chlorine type into again and use, the exchange capacity of this ion-exchange fiber is 2.0mmol/g.
ZL201110391576.1 discloses a kind of syrup decolorization method, use ion-exchange fiber, ion-exchange fiber is made taking polypropylene fibre as matrix, and decolouring concrete steps are: (1) with the distilled water preheating ion-exchange fiber post of 70～90 DEG C, the flow direction from bottom to top; (2) syrup, from bottom to top successively through the decolouring of first step anion-exchange fibre post, second stage cation-exchange fiber column desalination, the decolouring of third stage anion-exchange fibre post, obtains the syrup of decolouring.
Summary of the invention
The present invention is based on ion-exchange fiber and process the feature of the clear juice of cane sugar factory, in order to make the quality index of juice clearly meet the production requirement of refined sugar, realize One-step production refined sugar, on the basis of existing traditional technology, increase ion-exchange process, the quality index of syrup is improved, research adopts the new approach of One-step production refined sugar, and a kind of method of ion-exchange fiber efficient decolorizing One-step production refined sugar is provided.
The method of ion-exchange fiber efficient decolorizing One-step production refined sugar of the present invention, comprises the steps:
1) by the syrup pre-treatment of sulfurous method sugaring and carbonatation process sugaring gained;
2) carry out three grades of post exchange decolourings of male-female-the moon with ion-exchange fiber, to reaching refining sugar juice requirement, be collected in juice case clearly;
3) unload sugar: the residual sugar in the ion-exchange fiber exchange column after clear water cleaning is saturated, is recycled to juice case clearly;
4) the refining sugar juice of evaporation;
5) boil sugar: also comprise with white sugar do bed material with improve purity;
6) crystallization in motion, purging.
The present invention is after decolouring, and the clear juice that meets refined sugar requirement proceeds to subsequent disposal according to step process, simultaneously in order to produce linking, also needs using the ion-exchange fiber after for some time to regenerate.Thereby the present invention also comprises step 7) and step 8) described regeneration.
7) use the combination solution of NaCl solution or NaCl+HCl to the regeneration of second stage cation exchange fibre, use NaCl solution and/or CaCl
2solution is regenerated to the first step, third stage anion-exchange fibre;
8) the ion-exchange fiber exchange column after clear water cleaning and regeneration, till reaching neutrality to the water of discharging.
Step 1 of the present invention) described sulfurous method is refined sugar and the syrup of carbonatation process sugaring gained comprises: purified juice and the subsider juice of sulfurous method sugaring gained, a clear juice, two clear juice and the purified juices of carbonatation process sugaring gained.
Step 1) described pre-treatment comprises: first filters through the strainer of aperture 1～10 μ m, then filters through fabric filter; Fiber in fabric filter is identical with the fiber of ion-exchange fiber exchange column.The material such as mud, bagasse in syrup can be attached on fiber top layer, makes fibre agglomerates, and colloidalmaterial can be attached on the top layer of fiber to hinder exchange and the regeneration of pigment, so mud, bagasse, colloidalmaterial etc. must be removed before exchange.
In step 2), the wet volume density of anion-exchange fibre is 0.15～0.25g/cm
3, complete exchange capacity>=3.0 milligramequivalent/gram, the wet volume density of cation exchange fibre is 0.15～0.38/cm
3, complete exchange capacity>=4.0 milligramequivalent/gram.
In step 2), ion-exchange fiber exchange column adopts stainless steel column, ion-exchange fiber exchange filling aspect ratio is: 0.25～20, ion-exchange fiber packing density is: 80～120g/ml, pan feeding PH is 6～8, the temperature of decolouring is 25～100 DEG C, and when decolouring, syrup flow velocity is 10～100ml/min.
As preferred version, in step 2), ion-exchange fiber exchange filling aspect ratio is: 10～15, pan feeding PH is 6.8～7.4, and the temperature of decolouring is 65～80 DEG C, and when decolouring, syrup flow velocity is 40～60ml/min.
The present invention is in step 3), the clear water temperature of unloading sugared use is 70～80 DEG C.
Because purity of clear juice after above-mentioned steps only has 86～88%, with the sugaring of low-purity material boiling high purity extractive, be very difficult, therefore need to carry out boiling with high purity bed material.The present invention is in step 5), make bed material to improve purity to 90%～97% with one-level or top grade or refining white sugar.In clear juice, add one-level or top grade or refining white sugar, total purity is brought up to 90%～97%.So just can successfully make satisfactory refined sugar.
The present invention is in step 7), NaCl strength of solution is 5～15%, combination solution concentration is 5～15%NaCl+1%HCl, CaCl
2strength of solution is 1～10%, and temperature when regeneration is 20～90 DEG C, and the recovery time is 20～60 minutes, and the flow direction of regenerated liquid flows to contrary with syrup.In step 8), clear water temperature is 70～80 DEG C.
The present invention confirms, the combination regeneration effect of NaCl+HCl is best, merely with NaCl regeneration or all poor than the regeneration effect with NaCl+HCl by other combination its effect of regenerating.When regeneration, add after NaCl, first discharge yellow pigment, add after hydrochloric acid, have immediately a large amount of melanochrome to discharge, fiber bleaches immediately, and the regeneration effect of this explanation fiber is obvious, and the pigment of absorption is easy to wash-out.
Further preferably, in step 7), NaCl strength of solution is that 8～12%, CaCl2 strength of solution is 3～5%, temperature when regeneration is 70～80 DEG C.
In order to obtain better regeneration effect, also in order to make full use of regenerated liquid, reduce discharge, the present invention is in step 7), use the regeneration waste liquid of cation regenerant exchange fiber discharge and the regeneration waste liquid of anion regenerant exchange fiber discharge to regenerate in advance to anion-exchange fibre; Reclaiming third stage regeneration waste liquid regenerates in advance to first step anion-exchange fibre.
Decoloring method in the present invention and process and equipment, assembling mode etc. are all disclosed identical with ZL201110391576.1, that is: the preheating of ion-exchange fiber exchange column or cleaning pump into juice clearly after completing, successively through the decolouring of first step anion-exchange fibre, second stage cation exchange fibre desalination, the decolouring of third stage anion-exchange fibre, syrup is from bottom to top successively by each exchange column, and the clear juice after decolouring reaches refining sugar juice quality index and enters subsequent handling.
Solve the problem of fibre leakage and solve the aspect such as homogeneity question of exchange column also identical: in every joint exchange fiber 80 object stainless steel plates are installed up and down, 120 object stainless (steel) wires of liner, at 100 object stainless steel meshs of all outlet ports place liner, every segmented column ensures steadily while installation.The installation of fiber adopts hygrometric state filling, when filling, flattens and compresses.
In addition, in method of the present invention, the refining sugar juice of evaporation, the operation of boiling the operations such as sugar, crystallization in motion, purging can adopt the method for prior art.
Method of the present invention has following feature:
(1) design segment type exchange column, ensures the homogeneity that fiber loads.
(2) adopt stagewise desalination, the quality that ensures the clear juice of the decolouring requirement that touches the mark.
(3) adopt stainless steel column, the temperature while ensureing exchange.
(4) adopt and enter juice mode from bottom to top, the homogeneity while ensureing clear juice exchange and the clear mobile homogeneity of juice.
(5) adopt top-down regeneration enter material way, ensure regeneration thoroughness, avoid the secondary pollution of fiber.
(6) use falling film evaporator evaporation, effective.
(7) make bed material to improve purity, the sugaring of boiling high purity extractive with white sugar.
Facts have proved, for two step method, method of the present invention is saved back dissolving and double evaporation-cooling crystallisation process, can save 160 yuan of energy consumptions for ton sugar, save 0.15 ton, mark coal, for 300 tons of sugared small-sized sugar refinery of a daily output, 45 tons, mark coal can be saved every day, 4500 tons, mark coal can be saved every squeezing season; For one 600 tons sugared medium-sized sugar refinery, can save nearly 1000 tons of mark coal every squeezing season; And for for one 1000 tons sugared medium-sized sugar refinery, can save nearly 1500 tons of mark coal every squeezing season; For the sugared great Sheng of whole product Guangxi, as produce 1000000 tons of refined sugars per year, can save every year nearly 150,000 tons of mark coal, directly save 1.8 hundred million yuan of energy consumptions; Alleviate the pressure of atmosphere improvement, desulphurization denitration simultaneously.
On the other hand, in two step method, be applied to carbon and fill operation, can produce alkaline mud, cannot fully utilize, need landfill, and this technique is not used carbon to fill operation, without alkaline mud processing.
This technique has following features:
(1) ion-exchange fiber is not temporary transient inhibition to the removal effect of pigment, but fundamentally removes the base that adds lustre to.
(2) ion-exchange fiber is quite obvious to the decolorizing effect of clear juice, and the clear juice that decolours is superior, stable.
(3) easily, the recovery time is short in regeneration.The regeneration of use calcium salt, can not form pollution.
(4) ion-exchange fiber exchange velocity is fast, can meet sugar refinery scale operation demand.Ion-exchange fiber exchange capacity is large, can meet a large amount of and demand of high density pigment of removing in syrup.
(5) can be sugar refinery and increase by 96 yuan/ton of sugar of benefit.
(6) the recyclable regeneration of regeneration waste liquid.
(7) ion-exchange fiber long service life, can be used 2 to squeeze season, can meet sugar refinery and squeeze season requirement.
(8) strong adaptability to clear juice, can meet the demand of sugar refinery fluctuation.
(9) simple, the dependable performance of determined processing unit, has natural activity and can meet processing requirement.
(10) production that fixed technology condition and processing unit can be steady in a long-term, the performance index of clear juice have reached the quality control standards (QCS) that plan target requires.
(11) quality of raising sugar refinery product: the clear juice of producing by this technique can be directly used in production refined sugar completely, and the most of sugar refinery of China can only produce top grade sugar and first sugar, can not refined sugar processed, can Integral lifting sugar manufacturing industry product quality by realizing cane sugar factory single stage method refined sugar processed after this technique, increase China's sugar-refining industry competitive power in the world, will bring good economic benefit simultaneously.
(12) save energy: sugar industry is big power consumer, China is by the energy-conservation consequence of mentioning at present, and along with the raising of people's living standard, refined sugar production quantity will increase sharply.This technique is directly produced refined sugar from sugarcane and is become possibility, and the refined sugar technological process of production is simplified, and traditional sugar refining technology needs back dissolving to be cooked into raw sugar (consume approximately 18～20% pairs of sugarcane ratios of steam).
Comprehensive, the method of ion-exchange fiber efficient decolorizing One-step production refined sugar of the present invention, on the basis of existing tradition sugaring operation, increase ion fiber exchange operation, changing two step method is single stage method, directly utilizes the syrup of sulfurous method sugaring and carbonatation process sugaring gained to make refined sugar, and technique is simple, the quality index of syrup is improved, good product quality, and save energy, reduce environmental pollution.
Brief description of the drawings
Fig. 1 is the process flow sheet of ion-exchange fiber efficient decolorizing One-step production refined sugar.
Fig. 2 is the decolouring usefulness figure of different syrups.
Fig. 3 is the influence curve figure of temperature to adsorption.
Embodiment
Embodiment 1
The Decolorant Test of ion-exchange fiber to sub-method syrup
Purified juice and subsider juice that sulfitation sugar mill is chosen in test carry out static state decolouring simultaneous test, and test-results is shown in Fig. 2.As can be seen from Figure 2, ion-exchange fiber to the percent of decolourization of subsider juice apparently higher than purified juice, purified juice is to mix through subsider juice and filtered juice, purified juice contains more suspended substance than subsider juice, suspended substance easily covers the surface of fiber, and ion exchange process is to carry out on surface, suspended substance has stoped ion-exchange and adsorption bleaching process, and its decolouring usefulness to subsider juice is declined.Therefore, utilize ion-exchange fiber to decolour to syrup, should avoid the particularly pollution of colloid of suspended substance as far as possible.
Embodiment 2
The Decolorant Test of ion-exchange fiber to carbon method syrup
The decolorizing effect simultaneous test of anion-exchange fibre to the various syrups of carbon method, the results are shown in Table 1.
Table 1
Test-results shows, obvious to two clear juice decolorizing effects, treatment capacity is large.
Embodiment 3
The impact of temperature on two clear juice decolouring usefulness
Get 20g fiber (wetting), two clear juice, by the cooling or adjusting temperature of heating, are reacted and survey its colour after 30 minutes, the results are shown in Figure 3.
As can be seen from Figure 3, ion-exchange fiber to the optimum temperature range of sugar juice decoloring between 65～80 DEG C, more than 80 DEG C, along with the rising percent of decolourization of temperature slightly declines, this is because decolorization belongs to absorption exchange process, belong to chemisorption, between the active site on ion-exchange fiber surface and solute, there is Chemical bond, produce transfer transport phenomenon, absorption exchange process is mainly thermopositive reaction, temperature has certain influence to exchange process, it is stronger when temperature is low, when temperature is high a little less than, and temperature when high molecular motion more also weakened adsorption.And this optimum temperature range is the technological control temperature scope of two clear juice just, this explanation ion-exchange fiber is used in that two clear juice are decoloured is rational.
Embodiment 4
The impact of different aspect ratio on decolouring usefulness
Aspect ratio=loading height/diameter. different aspect ratio on decolouring impact in table 2.
Table 2
| Fibre weight (g) | Flow velocity (ml/min) | Aspect ratio | Treatment capacity (ml) | Colour (° St) |
| 30 | 50 | 14.5 | 1000 | 4 |
| 30 | 50 | 14.5 | 2000 | 7 |
| 30 | 50 | 14.5 | 3000 | 8 |
| 30 | 80 | 0.6 | 1000 | 5 |
| 30 | 80 | 0.6 | 2000 | 7 |
| 30 | 80 | 0.6 | 3000 | 9 |
| 30 | 100 | 0.25 | 1000 | 6 |
| 30 | 100 | 0.25 | 2000 | 7 |
| 30 | 100 | 0.25 | 3000 | 8 |
Table 2 can find out, when aspect ratio is 14.5, when flow velocity is 50ml/min, decolorizing effect is best, now, increases loading height, just increased the duration of contact of syrup and fiber surface, thus increase decolorizing effect.
Embodiment 5
Regeneration test
Test method: fill 15 grams of anion-exchange fibres in the glass column of two Φ 20 × 400, process clear juice 900ml at every turn, adopt different concns and different regenerators to regenerate.
Test-results:
(1) calcium chloride concentration: 5%, sodium chloride concentration: 5%. the results are shown in Table 3.
Table 3
| Sample title | Colour (IU) | Percent of decolourization (%) |
| Former clear juice | 2121 | ? |
| The calcium chloride rear decoloring for the first time of regenerating | 127 | 94.01 |
| The sodium-chlor rear decoloring for the first time of regenerating | 225 | 89.39 |
| The calcium chloride rear decoloring for the second time of regenerating | 166 | 92.17 |
| The sodium-chlor rear decoloring for the second time of regenerating | 201 | 90.52 |
| The calcium chloride rear decoloring for the third time of regenerating | 140 | 93.40 |
| The sodium-chlor rear decoloring for the third time of regenerating | 164 | 92.27 |
| The 4th rear decoloring of calcium chloride regeneration | 206 | 92.96 |
| The 4th rear decoloring of sodium-chlor regeneration | 211 | 90.05 |
| The 5th rear decoloring of calcium chloride regeneration | 240 | 88.68 |
| The 5th rear decoloring of sodium-chlor regeneration | 252 | 88.12 |
| The 6th rear decoloring of calcium chloride regeneration | 251 | 88.17 |
| The 6th rear decoloring of sodium-chlor regeneration | 263 | 87.60 |
Can find out by test, the regeneration effect of the calcium chloride of equal in quality concentration is obviously better than the regeneration effect of sodium-chlor.
(2) the calcium chloride regeneration test of different concns
Along with the rising of concentration, regeneration effect is become better and better, and the pigmentary colours that wash out are more and more darker.The results are shown in Table 4.
Table 4
| Sample title | Colour/IU | Percent of decolourization |
| Former clear juice | 2458 | ? |
| 1% calcium chloride regeneration rear decoloring | 212 | 91.38 |
| 2% calcium chloride regeneration rear decoloring | 187 | 92.39 |
| 3% calcium chloride regeneration rear decoloring | 179 | 92.720 |
| The 4th rear decoloring of 5% calcium chloride regeneration | 162 | 93.41 |
| The 4th rear decoloring of 10% calcium chloride regeneration | 140 | 94.30 |
(3) the tired longevity test of ion-exchange fiber
Investigate ion-exchange fiber Reusability and regeneration exchange capacity decline degree afterwards.The results are shown in Table 5.
Table 5
From fatigue test results, anion-exchange fibre exchange capacity after using 310 times declines 7.3%, be greater than 310 the work-ing life of this explanation anion-exchange fibre, simultaneously exchange capacity is too in the time using after 400 exchange capacities and dispatch from the factory for cation exchange fibre, without declining, cation exchange fibre was greater than 400 times in work-ing life, and this explanation ion-exchange fiber can use 2 to squeeze season for the treatment of the clear juice of cane sugar factory completely.
Embodiment 6
Sugar refinery test
In order to make refined sugar, show that by Test Summary the technical indicator that after decolouring, juice finally will reach is clearly as shown in table 6.
Table 6
| Sequence number | Project name | Index | Remarks |
| 1 | Gravity purity/(%) | ≥85 | ? |
| 2 | Gravity purity is poor/(%) | ≥1 | Compared with clear juice |
| 3 | PH value | 7.0～8.0 | ? |
| 4 | Temperature/(DEG C) | 70～80 | ? |
| 5 | Turbidity/(MAU) | ≤20 | ? |
| 6 | Calcium salt/(%OBX) | 0.072 | ? |
| 7 | Decalcification rate/(%) | ≥84 | Compared with clear juice |
| 8 | Sucrose/(%) | Remain basically stable with clear juice Sucrose | ? |
| 9 | Reducing sugar/(%) | A little less than clear juice reducing sugar content | ? |
| 10 | Colour | ≤ 180IU or≤15 ° of St | ? |
| 11 | Percent of decolourization (%) | ≥84％ | Compared with clear juice |
The physical and chemical index of refined sugar should meet GB317-2006 requirement, as shown in table 7.
Table 7
The present embodiment, main raw material(s) is ZB-1 cation exchange fibre and ZB-2 anion-exchange fibre, and main chemical raw material adopts technical grade, and water adopts water of condensation, specifically in table 8.ZB series is taking polypropylene (PP) fiber as matrix, the ion-exchange fiber of preparing by introducing quaternary amine base after irradiation grafting.
Table 8
The variation of pilot scale various process parameters, the every quality index variation of clear juice, clear juice quality change situation are respectively in table 9,10,11.
Table 9
Table 10
As can be seen from Table 10, clear juice steady quality after the first segmented column, the second segmented column, the 3rd segmented column successively, colour reduces successively, and clear juice is from Section three is discharged, and colour raises successively, and during to 180IU, treatment capacity is 2m
3time saturated, colour declines rapidly.
Table 11
From upper table 11, decolouring rear decoloring rate is equal more than 90%, and colour is lower than 200IU.Purity also raises to some extent in addition, but can't reach refined sugar requirement, boils sugar so need to throw bed material.
After the inventive method is processed, each operation material colour the results are shown in Table 12.
Table 12
To make to decolour color value of clear juice lower than 200IU through decolouring, then boiling five tank refined sugars (6 tons), two tank high-quality sugar (2.4 tons), quality product all meets project check requirement.
In resin container, load 7m
3(2 tons) ion-exchange fiber, has moved 3 hours continuously, pervaporation separately, and boiling pan boils sugar, and one day tank is prepared 2 tank refined sugars altogether, and product out meets the requirement of refined sugar completely, adds up to 52 tons.White Sugar Quality assay is as table 13.
Table 13
| Sequence number | Interventions Requested | Standard-required | Assay | Conclusion |
| 1 | Sucrose (%) | ≥99.8 | 99.8 | Qualified |
| 2 | Reducing sugar content (%) | ≤0.03 | 0 | Qualified |
| 3 | Electricity is led ash content (%) | ≤0.02 | 0.002 | Qualified |
| 4 | Weight loss on drying (%) | ≤0.06 | 0.02 | Qualified |
| 5 | Colour (IU) | ≤25 | 16 | Qualified |
| 6 | Turbidity (MAU) | ≤30 | 2 | Qualified |
| 7 | Water insoluble impurity (mg/kg) | ≤10 | 2 | Qualified |
Standard-required is according to GB317-2006.
Claims (10)
1. the method for ion-exchange fiber efficient decolorizing One-step production refined sugar, comprises the steps:
1) by the syrup pre-treatment of sulfurous method sugaring and carbonatation process sugaring gained;
2) carry out three grades of post exchange decolourings of male-female-the moon with ion-exchange fiber, to reaching refining sugar juice requirement, be collected in juice case clearly;
3) unload sugar: the residual sugar in the ion-exchange fiber exchange column after clear water cleaning is saturated, is recycled to juice case clearly;
4) the refining sugar juice of evaporation;
5) boil sugar: comprise with white sugar do bed material with improve purity;
6) crystallization in motion, purging.
2. method according to claim 1, is characterized in that: also comprise:
7) use the combination solution of NaCl solution or NaCl+HCl to the regeneration of second stage cation exchange fibre, use NaCl solution and/or CaCl
2solution is regenerated to the first step, third stage anion-exchange fibre;
8) the ion-exchange fiber exchange column after clear water cleaning and regeneration, till reaching neutrality to the water of discharging.
3. method according to claim 1, it is characterized in that: step 1) described sulfurous method is refined sugar and the syrup of carbonatation process sugaring gained comprises: purified juice and the subsider juice of sulfurous method sugaring gained, a clear juice, two clear juice and the purified juices of carbonatation process sugaring gained; Described pre-treatment comprises: first filter through the strainer of aperture 1～10 μ m, then filter through fabric filter; Fiber in fabric filter is identical with the fiber of ion-exchange fiber exchange column.
4. method according to claim 1, is characterized in that: in step 2), the wet volume density of anion-exchange fibre is 0.15～0.25g/cm
3, complete exchange capacity>=3.0 milligramequivalent/gram, the wet volume density of cation exchange fibre is 0.15～0.38g/cm
3, complete exchange capacity>=4.0 milligramequivalent/gram.
5. method according to claim 1, it is characterized in that: in step 2), ion-exchange fiber exchange column adopts stainless steel column, ion-exchange fiber exchange filling aspect ratio is: 0.25～20, ion-exchange fiber packing density is: 80～120g/ml, pan feeding PH is 6～8, and the temperature of decolouring is 25～100 DEG C, and when decolouring, syrup flow velocity is 10～100ml/min.
6. method according to claim 1 or 5, is characterized in that: in step 2), ion-exchange fiber exchange filling aspect ratio is: 10～15, pan feeding PH is 6.8～7.4, and the temperature of decolouring is 65～80 DEG C, and when decolouring, syrup flow velocity is 40～60ml/min.
7. method according to claim 1, is characterized in that: in step 3), the clear water temperature of unloading sugared use is 70～80 DEG C; In step 5), make bed material to improve purity to 90%～97% with one-level or top grade or refining white sugar.
8. method according to claim 2, is characterized in that: in step 7), NaCl strength of solution is 5～15%, combination solution concentration is 5～15%NaCl+1%HCl, CaCl
2strength of solution is 1～10%, and temperature when regeneration is 20～90 DEG C, and the recovery time is 20～60 minutes, and the flow direction of regenerated liquid flows to contrary with syrup;
In step 8), clear water temperature is 70～80 DEG C.
9. according to the method described in claim 2 or 8, it is characterized in that: in step 7), NaCl strength of solution is 8～12%, CaCl
2strength of solution is 3～5%, and temperature when regeneration is 70～80 DEG C.
10. method according to claim 2, is characterized in that: in step 7), use the regeneration waste liquid of cation regenerant exchange fiber discharge and the regeneration waste liquid of anion regenerant exchange fiber discharge to regenerate in advance to anion-exchange fibre; Reclaiming third stage regeneration waste liquid regenerates in advance to first step anion-exchange fibre.
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| CN112593016A (en) * | 2020-12-22 | 2021-04-02 | 新疆冠农果茸股份有限公司 | Process for preparing high-quality white granulated sugar and fulvic acid dry powder from beet |
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| CN102492781A (en) * | 2011-12-01 | 2012-06-13 | 桂林正翰科技开发有限责任公司 | Syrup decolorization method |
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