CN102319592B - Method for preparing inorganic potassium salt based on sugar making diethyl ether and dilute juice desalination - Google Patents
Method for preparing inorganic potassium salt based on sugar making diethyl ether and dilute juice desalination Download PDFInfo
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- CN102319592B CN102319592B CN2011101395264A CN201110139526A CN102319592B CN 102319592 B CN102319592 B CN 102319592B CN 2011101395264 A CN2011101395264 A CN 2011101395264A CN 201110139526 A CN201110139526 A CN 201110139526A CN 102319592 B CN102319592 B CN 102319592B
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Abstract
The invention discloses a method for preparing an inorganic potassium salt based on sugar making diethyl ether and dilute juice desalination. The method comprises the following steps of: (1) eluting a resin bed with sodium strong acid cation exchange resin and diethyl ether to obtain potassium-saturated depotassication resin and depotassication diethyl ether; (2) eluting the resin bed with the depotassication resin obtained in the step (1) and a sodium sulfate solution to obtain sodium strong acid cation exchange resin and potassium-containing eluent; (3) eluting the resin bed with the sodium strong acid cation exchange resin and sugar making dilute juice to obtain calcium-saturated decalcification resin and decalcification dilute juice; (4) eluting the resin bed with the calcium-saturated decalcification resin obtained in the step (3) and the depotassication diethyl ether obtained in the step (1) to obtain sodium strong acid cation exchange resin and depotassication sodium diethyl ether; and (5) preparing an inorganic potassium salt from the potassium-containing eluent. According to the method, the content of potassium and sodium in the diethyl ether and the content of calcium in the dilute juice are lowered, the scaling of an evaporating pot is reduced, and a crystallized inorganic potassium salt with a high added value is prepared simultaneously.
Description
Technical field
The present invention relates to make in the sugar industry sugaring second honey de-kalium-sodium and the dilute juice decalcification technology of spent ion exchange resin, particularly regeneration of resin and inorganic potassium salt novel preparation method thereof belong to the Sugar Engineering field.
Background technology
Potassium is one of three big nutrients of decision agricultural high yield.Potassium element in 2005 reaches 2000～2,500 hundred million yuan to the contribution of China's GDP, accounts for 20%～30% of GDP total amount, and wherein 95% is as the increasing both production and income of potash fertilizer to crops.China is as large agricultural country, but the resource potassium deficiency, sylvite is one of China's two kinds of nonmetallic minerals the most in short supply.By 2005, Chinese sylvite reserves were amounted to K
2O is 8291.6 ten thousand tons, only accounts for world's gross reserves about 1%.Existing sylvite supply far can not be satisfied the China's national economy development need, and main dependence on import: 2007, Chinese import potash fertilizer was amounted to K
2O is 597.2 ten thousand tons, accounts for 71.8% of aggregate consumption.
In beet sugar manufacture, owing to reasons such as the use of fertilizer and soil mineralizations, potassium and sodium content are very high in the beet, K in the second honey that causes refining sugar
+And Na
+Content respectively up to 2% (w/w) and 1% (w/w).But K
+And Na
+Be to make mellite, its a large amount of existence can significantly be reduced sugar total recovery.In juice,liming or peace and quiet operation, need to add a large amount of lime simultaneously as nertralizer and fining agent, because Ca
2+Clarify not thoroughly, cause residual a large amount of calcium salts in the syrup, reach 100～500mg/L (in CaO), a large amount of calcium salts can cause evaporator incrustation, reduces heat conductive efficiency and increases and makes sweet coefficient, thereby reduce sugar total recovery.In cane sugar manufacture second honey and dilute juice (being clear juice), also be rich in alkali metal and calcium salt respectively, give the Closed Circulation in Sugar Production deleterious impact.Therefore reducing in the second honey potassium sodium and dilute juice calcium salt content is an important production technology management work, and realizes that the high-valued utilization of resources of potassium can partly alleviate china natural resources property potassium deficiency problem.
Traditional second honey de-kalium-sodium method is the Quntin method, promptly with Mg
2+Type ion exchange resin takes off K to second honey
+, Na
+, to make the low Mg of sweet coefficient
2+Replace making the high K of sweet coefficient
+, Na
+But, a large amount of MgCl of needs when the Quntin method is used for the second honey de-kalium-sodium
2Cook regenerative agent.Chinese patent 200510094368.X has announced a kind of softening, desalination, dealkalize, decolouring and refining device of beet liquid glucose; Can reach better desalination, decolorizing effect; But its technological process is very complicated, and needs in the operating process to use a large amount of chemical reagents, and security can not guarantee.Chinese patent 200910040830.6 announced and a kind ofly prepared the method for inorganic sylvine crystal and feed addictive with cane molasses fermentation alcohol waste liquid, but its to select resin for use be H
+Type ion exchange resin is intended to sylvite in the recovered alcohol waste liquid.If select H for use
+Desalination can cause then that sucrose transforms in the molasses to type ion exchange resin under acid condition to second honey, influences the sugar recovery equally.Aspect the dilute juice decalcification, using more at present is to utilize cationic ion-exchange resin to the syrup decalcification, and effect also very significantly.But this method also has very big shortcoming, needs a large amount of salt to make regenerative agent, and gets into the Na in the syrup
+And Cl
-All belong to and make mellite, the molasses amount is increased, the sucrose loss increases, and also producing a large amount of regenerative wastewater simultaneously needs to handle.Have bibliographical information electroosmose process capable of using that syrup is carried out decalcification, have good decalcification effect, the decalcification rate reaches 99%, but power consumption is high, handle syrup concentration and temperature all is restricted.Applicant's Chinese invention patent 200810218805.8 has been announced a kind of renovation process of di-mix honey de-kalium-sodium resin; Prepare calcium type resin with dilute juice or dilute juice electroosmose process decalcification waste water; To the second honey de-kalium-sodium, the method has good application scenario again, but that existing problems are calcium concentrations in the dilute juice is too low; Be not enough to second honey in potassium sodium exchange, the potassium content in the second honey is very high but not to obtain the utilization of resources.
Summary of the invention
The objective of the invention is to overcome the prior art deficiency; Regeneration of ion-exchange resin waste water pollution problem to sugaring second honey de-kalium-sodium, dilute juice decalcification provides a kind of inorganic potassium salt preparation method based on the decalcification of second honey de-kalium-sodium dilute juice, takes off the potassium resin with metabisulfite solution regeneration; Recycling contains the potassium regeneration liquid waste; And prepare inorganic potash fertilizer, to take off potassium second honey regeneration decalcification resin, obtain sodium type resin and take off potassium sodium second honey then; The pollution-free regeneration of potassium and decalcification resin is taken off in realization, reduces the inorganic sylvine crystal of potassium sodium content in the second honey, the fouling of minimizing evaporator, preparation high added value.Be issued in the condition that does not produce regeneration liquid waste that inorganic potassium salt extracts, the purpose of dilute juice decalcification and second honey de-kalium-sodium, technical scheme of the present invention is specific as follows:
A kind of inorganic potassium salt preparation method based on sugaring second honey and dilute juice desalination comprises the steps:
(1) sugaring second honey takes off potassium: it is sodium type strong-acid cation-exchange resin that the potassium resin is taken off in employing; Hammer degree, temperature and the treating capacity of second honey are controlled at 40～65 ° of Bx, 60～85 ℃ and 80～120L respectively; And with 1～3BV/h flow velocity wash-out resin bed of (BV representes the resin bed volume, and 1BV=20L is together following); Do not have potassium with demineralized water backwash resin bed to water outlet again, get saturated the taking off the potassium resin and take off potassium second honey of potassium;
(2) wash-out of potassium: the potassium resin that takes off that adopts step (1) to obtain is an exchanger resin; Adopting metabisulfite solution (glauber salt) is regenerative agent; Regenerative agent concentration and consumption are controlled at respectively in the scope of 80～125g/L and 32～50L, and temperature is controlled at 50～85 ℃, with the flow velocity wash-out resin bed of 1～3BV/h; Do not have potassium with demineralized water backwash resin bed to water outlet again, obtain sodium type strong-acid cation-exchange resin and contain the potassium eluent; The potassium resin that takes off after the regeneration is used for next round second honey and takes off potassium and resin regeneration circulation, contains the potassium regeneration liquid waste and can be used to prepare inorganic potassium salt;
(3) decalcification of dilute sugar juice: adopt the ion-exchange decalcification, the decalcification resin is a sodium type strong-acid cation-exchange resin, and the dilute sugar juice consumption is 1440L～7200L, wherein Ca
2+Concentration is counted 100～500mg/L with CaO, and temperature is controlled at 60～85 ℃, and dilute sugar juice through resin bed, does not have calcium with demineralized water backwash resin bed to water outlet with 5～10BV/h flow velocity again, obtains saturated decalcification resin of calcium and decalcification dilute juice;
(4) wash-out of calcium: the saturated decalcification resin of calcium that adopts step (3) to obtain is an exchanger resin; Regenerative agent be step (1) obtain take off potassium second honey; The regenerative agent temperature is controlled at 60～85 ℃, and consumption is controlled in the scope of 80～120L, with the flow velocity wash-out resin bed of 2～3BV/h; Again with demineralized water backwash resin bed to going out water colorless, obtain sodium type strong-acid cation-exchange resin and take off potassium sodium second honey; Gained sodium type resin is used for the dilute juice decalcification or second honey takes off potassium, takes off potassium sodium second honey and is used for three sand and boils sugar.Take off the renewable decalcification resin of potassium second honey according to being: Na in the second honey
+Concentration is up to 1～2%, Na during second honey takes off behind the potassium
+Content further increases, and makes molecular balance
(R represents resin) moves right, and helps Ca
2+Get into liquid phase, realize Na
+And Ca
2+Exchange.
(5) the potassium eluent that contains that obtains with step (2) prepares inorganic potassium salt.
Preferably, step (1) and (3) said sodium type strong-acid cation-exchange resin are BK001.
Preferably; Step (1) and (3) said sodium type strong-acid cation-exchange resin also pass through following preliminary treatment: the 20L resin is used earlier distilled water immersion 12h; Washing resin to water outlet free from admixture; Use 80L concentration respectively to handle 2h as the 1M sodium hydroxide solution then respectively, all be washed till pH neutrality after each the processing with distilled water as 1M hydrochloric acid and 80L concentration.
Preferably, the preparation method of said inorganic potassium salt: collect variable concentrations and contain the potassium eluent, adjusting its hammer degree is 15～20 ° of Bx; In 0～40 ℃ evaporating, concentrating and crystallizing jar; With 150～250rpm rotating speed stirred crystallization, the brilliant cream of gained potassium sulfate is through separating gained K through the filter paper suction filtration
2SO
4Crystal promptly gets crystalline sulfuric acid potassium 40～60 ℃ of forced air dryings.
The present invention compared with prior art has following advantage:
(1) utilization of the present invention is taken off potassium second honey and is regenerative agent, with its regeneration sugaring decalcification resin, obtains sodium type resin and takes off potassium sodium second honey, and gained sodium type resin can be used for the dilute juice decalcification or second honey takes off potassium, takes off potassium sodium second honey and can be used for three sand and boil sugar.Promptly realize the green regenerating of decalcification resin, carried out taking off sodium to taking off potassium second honey again, obtained taking off potassium sodium second honey.
(2) the present invention utilizes to reclaim and contains the potassium eluent, utilizes the method for evaporating, concentrating and crystallizing to prepare a kind of inorganic potassium salt, and the potassium ion crystallization rate of recovery (mass fraction) approximately is 85%.Because of the source of its potassium is a potassium ion residual in the second honey, has reduced on the one hand and has made the maximum K of sweet coefficient in the second honey
+Concentration helps the recovery of sugar;
Find a kind of new method for preparing inorganic potassium salt on the other hand again.
(3) among the present invention second honey through taking off potassium and taking off the K that makes sweet coefficient maximum after processings such as sodium in the second honey
+Concentration reduces 53.7%, makes the bigger Na of sweet coefficient
+Concentration increases by 31.1%, makes the minimum Ca of sweet coefficient
2+Concentration has then increased by 3.75 times. and to helping the direction variation that sugar reclaims, second honey quality increases second honey after treatment generally.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further detailed description, but embodiment of the present invention is not limited thereto.
Embodiment 1
As shown in Figure 1, a kind of inorganic potassium salt preparation method based on sugaring second honey and dilute juice desalination may further comprise the steps: (1) sugaring second is sweet takes off potassium; (2) wash-out of potassium; (3) decalcification of system sugar juice; (4) wash-out of calcium; (5) the evaporative crystallization legal system is equipped with inorganic potassium salt.Concrete steps are following:
(1) sugaring second honey take off potassium: 20L sodium type strong-acid cation-exchange resin BK001 is used earlier distilled water immersion 12h; Washing resin to water outlet free from admixture; Use 80L concentration respectively to handle 2h as the 1M sodium hydroxide solution then, all be washed till neutrality after each the processing with distilled water as 1M hydrochloric acid and 80L concentration.Pretreated 20L BK001 resin wet method is inserted ion exchange column (among the Φ 0.15m * 2.00m); With temperature is that 75 ℃, hammer degree are that 57.3 ° of Bx and volume are that the beet-sugar factory second honey of 100L (being 5BV) passes through resin bed with the speed of 2BV/h; With the 100L demineralized water with the flow velocity backwash resin bed of 5BV/h to going out water colorless, potassium is saturated takes off the potassium resin and take off potassium second honey.
(2) wash-out of potassium: adopt the metabisulfite solution regeneration potassium of 100g/L saturated take off the potassium resin, regenerative agent temperature and consumption are respectively 70 ℃ and 40L, with the flow velocity wash-out resin bed of 2BV/h, it is subsequent use that collection contains the eluent of potassium.At this moment, the eluting rate of potassium is 85.8%.
(3) system sugar juice decalcification: with 20L sodium type strong-acid cation-exchange resin BK001 set by step (1) carry out preliminary treatment; Then pretreated 20L BK001 resin wet method is inserted another ion exchange column (among the Φ 0.15m * 2.00m); With 180 BV (3600L) temperature is 85 ℃ beet-sugar factory dilute juice, wherein Ca
2+Concentration is 270mg/L (in CaO), through resin bed, does not have calcium with demineralized water backwash resin bed to water outlet with the 8BV/h flow velocity again, gets saturated decalcification resin and the decalcification dilute juice of calcium.At this moment, dilute juice decalcification rate is more than 90%.
(4) wash-out of calcium: taking off potassium second honey with 100L is regenerated liquid, flows through the decalcification resin bed at 75 ℃ with the 2.5BV/h flow velocity, and the recovery time is 5h; With 100L is that 5BV demineralized water backwash resin bed is to going out water colorless.Obtain sodium type resin and take off potassium sodium second honey, gained sodium type resin can be used for the dilute juice decalcification or second honey takes off potassium, takes off potassium sodium second honey and can be used for three sand and boil sugar.At this moment, decalcification regeneration of resin rate is 92.4%.Realized the decalcification regeneration of resin and taken off potassium second honey continuing to take off sodium, made Ca in the dilute sugar juice
2+With take off Na in the potassium second honey
+Cross evaporator and realize exchanging, avoid Ca
2+Existence cause evaporator fouling and heat transfer efficiency to reduce, reduce in the second honey potassium sodium etc. and make mellite content and improve sugar total recovery.
(5) the evaporating, concentrating and crystallizing legal system is equipped with inorganic potassium salt: the hammer degree that contains the potassium regeneration liquid waste that step (2) is collected is adjusted to 15 ° of Bx; Crystallization temperature is 40 ℃; Rotating speed is crystallization in the evaporating, concentrating and crystallizing jar of 250r/min, and the brilliant cream of the potassium sulfate that obtains is earlier through separating through the filter paper suction filtration, then with gained K
2SO
4Crystal is dry under 50 ℃, promptly gets crystalline sulfuric acid potassium 986.3g.
The potassium ion crystallization rate of recovery is about 85% (mass fraction), gained K
2SO
4The crystal crystalline form is more complete, accounts for 80% of crystal total amount greater than 40 purpose crystal mass, is superior to the commercially available prod.
Embodiment 2
The difference of present embodiment and embodiment 1 is:
Change hammer degree, temperature and the treating capacity of second honey in the step (1) into 65 ° of Bx, 85 ℃ and 80L (being 4BV) respectively, the sample introduction flow velocity is 1BV/h.
The concentration of the metabisulfite solution in the step (2) is adjusted into 80g/L, and volume is 50L, 50 ℃ of operating temperatures, and flow velocity is 3BV/h.At this moment, the eluting rate of potassium is 87.2%.
Use Ca in the step (3)
2+Concentration is 100mg/L (in CaO) beet-sugar factory dilute juice, and its treating capacity is 360BV (7200L), and operating temperature is 60 ℃, and flow velocity is 10BV/h.At this moment, dilute juice decalcification rate is greater than 93%.
Taking off potassium second honey volume in the step (4) is 80L, under 85 ℃, flows through resin bed with the 2BV/h flow velocity, and the recovery time is adjusted into 4h.At this moment, decalcification resin regeneration rate becomes 94.3%.
The temperature of evaporating, concentrating and crystallizing jar is adjusted into 25 ℃ of room temperatures in the step (5); Contain potassium regeneration liquid waste hammer degree and be adjusted into 18 ° of Bx, agitator speed 200rpm, 60 ℃ of crystalline sulfuric acid potassium baking temperatures; Obtain crystalline sulfuric acid potassium 993.4g this moment, and the potassium ion crystallization rate of recovery is 86.4%.
Embodiment 3
The difference of present embodiment and embodiment 1 is:
Change the sugaring second honey in the step (1) into carbonic acid law cane sugar factory second honey, its dilution back hammer degree, temperature and treating capacity are respectively 40 ° of Bx, 60 ℃ and 120L (being 6BV), and the charging flow velocity is 3BV/h.
The concentration of the metabisulfite solution in the step (2) is adjusted into the metabisulfite solution into 125g/L, and regenerative agent temperature and consumption are respectively 85 ℃ and 32L, and flow velocity is 1BV/h.At this moment, the eluting rate of potassium is 88.3%.
Use Ca in the step (3)
2+Concentration is 500mg/L (in CaO) carbonic acid law cane sugar factory dilute juice (clear juice), and its treating capacity is 72BV (1440L), and temperature is 75 ℃, and flow velocity is 5BV/h.At this moment, clear juice decalcification rate is greater than 88.0%.
120L takes off potassium second honey and flows through resin bed at 60 ℃ with the 3BV/h flow velocity in the step (4), and the recovery time is 6h.At this moment, decalcification resin regeneration rate becomes 91.6%.
Step maintains the evaporating, concentrating and crystallizing jar in the ice-water bath in (5); Contain potassium regeneration liquid waste concentration and be adjusted into 20 ° of Bx; Crystallizing tank agitator speed 150rpm, crystalline sulfuric acid potassium crystal is 1013.6g 40 ℃ of dry backs to constant weight, the potassium ion crystallization rate of recovery is 88.1%.
The foregoing description is a preferred implementation of the present invention, and other any condition transformation and equivalent substitute mode of being done under thinking of the present invention and the principle that do not deviate from is included within protection scope of the present invention.
Claims (3)
1. the inorganic potassium salt preparation method based on sugaring second honey and dilute juice desalination is characterized in that, comprises the steps:
(1) sugaring second honey takes off potassium: it is sodium type strong-acid cation-exchange resin that the potassium resin is taken off in employing; Hammer degree, temperature and the treating capacity of second honey are controlled at 40～65 ° of Bx, 60～85 ℃ and 80～120L respectively; And with the flow velocity wash-out resin bed of 1～3BV/h; Do not have potassium with demineralized water backwash resin bed to water outlet again, get saturated the taking off the potassium resin and take off potassium second honey of potassium;
(2) wash-out of potassium: the potassium resin that takes off that adopts step (1) to obtain is an exchanger resin; The employing metabisulfite solution is a regenerative agent; Regenerative agent concentration and consumption are controlled at respectively in the scope of 80～125g/L and 32～50L, and temperature is controlled at 50～85 ℃, with the flow velocity wash-out resin bed of 1～3BV/h; Do not have potassium with demineralized water backwash resin bed to water outlet again, obtain sodium type strong-acid cation-exchange resin and contain the potassium eluent;
(3) decalcification of dilute sugar juice: adopt the ion-exchange decalcification, the decalcification resin is a sodium type strong-acid cation-exchange resin, and the dilute sugar juice consumption is 1440L～7200L, wherein Ca
2+Concentration is counted 100～500mg/L with CaO, and temperature is controlled at 60～85 ℃, and dilute sugar juice through resin bed, does not have calcium with demineralized water backwash resin bed to water outlet with 5～10BV/h flow velocity again, obtains saturated decalcification resin of calcium and decalcification dilute juice;
(4) wash-out of calcium: the saturated decalcification resin of calcium that adopts step (3) to obtain is an exchanger resin; Regenerative agent be step (1) obtain take off potassium second honey; The regenerative agent temperature is controlled at 60～85 ℃, and consumption is controlled in the scope of 80～120L, with the flow velocity wash-out resin bed of 2～3BV/h; Again with demineralized water backwash resin bed to going out water colorless, obtain sodium type strong-acid cation-exchange resin and take off potassium sodium second honey;
(5) the potassium eluent that contains that obtains with step (2) prepares inorganic potassium salt; The preparation method of said inorganic potassium salt: collect variable concentrations and contain the potassium eluent; Adjusting its hammer degree is 15～20 ° of Bx, in 0～40 ℃ evaporating, concentrating and crystallizing jar, with 150～250rpm rotating speed stirred crystallization; The brilliant cream of gained potassium sulfate is through separating gained K through the filter paper suction filtration
2SO
4Crystal promptly gets crystalline sulfuric acid potassium 40～60 ℃ of forced air dryings.
2. a kind of inorganic potassium salt preparation method based on sugaring second honey and dilute juice desalination according to claim 1 is characterized in that the said sodium type of step ⑴ and ⑶ strong-acid cation-exchange resin is BK001.
3. a kind of inorganic potassium salt preparation method according to claim 1 and 2 based on sugaring second honey and dilute juice desalination; It is characterized in that; The said sodium type of step ⑴ and ⑶ strong-acid cation-exchange resin also passes through following preliminary treatment: the 20L resin is used earlier distilled water immersion 12h; Washing resin to water outlet free from admixture uses 80L concentration respectively to handle 2h as 1M hydrochloric acid and 80L concentration as the 1M sodium hydroxide solution then respectively, all is washed till pH neutrality with distilled water after each the processing.
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|---|---|---|---|
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|---|---|---|---|
| CN2011101395264A CN102319592B (en) | 2011-05-27 | 2011-05-27 | Method for preparing inorganic potassium salt based on sugar making diethyl ether and dilute juice desalination |
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| CN102319592B true CN102319592B (en) | 2012-12-05 |
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| CN104030735A (en) * | 2014-07-07 | 2014-09-10 | 云南省轻工业科学研究院 | Preparation method of high-concentration water-soluble plant potash fertilizer |
| CN114277197A (en) * | 2021-10-22 | 2022-04-05 | 欧尚元(天津)有限公司 | Method for softening beet syrup |
| NL2031846B1 (en) | 2022-05-12 | 2023-11-20 | Biota Holding B V | Method for recovering nutrients from vegetable streams |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101403017A (en) * | 2008-10-31 | 2009-04-08 | 华南理工大学 | Regeneration method for di-mix honey de-kalium-sodium resin |
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|---|---|---|---|---|
| CN101403017A (en) * | 2008-10-31 | 2009-04-08 | 华南理工大学 | Regeneration method for di-mix honey de-kalium-sodium resin |
Non-Patent Citations (4)
| Title |
|---|
| A modified quentin method for desalting thin juice and mother liquor B in beet sugar industry;Siming Zhu et al.;《Desalination》;20101109;第268卷;第214-220页 * |
| BK001树脂对稀糖汁脱钙的工艺条件及反应动力学;杨璇璇等;《河南工业大学学报(自然科学版)》;20090630;第30卷(第3期);第48-51页 * |
| Siming Zhu et al..A modified quentin method for desalting thin juice and mother liquor B in beet sugar industry.《Desalination》.2010,第268卷第214-220页. |
| 杨璇璇等.BK001树脂对稀糖汁脱钙的工艺条件及反应动力学.《河南工业大学学报(自然科学版)》.2009,第30卷(第3期),第48-51页. |
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