CN101830817A

CN101830817A - Method for continuous multistage membrane separation of trimethylamine ethylene colactone from salt compound

Info

Publication number: CN101830817A
Application number: CN200910119286A
Authority: CN
Inventors: 刘驳谦
Original assignee: Individual
Current assignee: Individual
Priority date: 2009-03-12
Filing date: 2009-03-12
Publication date: 2010-09-15

Abstract

The invention discloses a method for continuous multistage membrane separation of a trimethylamine ethylene colactone from a salt compound, which comprises the following steps of: dividing aqueous solution of which the mass ratio of trimethylamine ethylene colactone to salt compound is or is proximate to a critical mass ratio into two parts, introducing the two parts into the first stage and the tail stage of a multistage membrane separation system in a continuous and opposite reverse flow way respectively, continuously obtaining high-salt concentration aqueous solution of the trimethylamine ethylene colactone, of which the mass ratio of the trimethylamine ethylene colactone to the salt compound is low to the largest extent and is less than the critical mass ratio, from the first stage of the multistage membrane separation system; and converting the high-salt concentration aqueous solution of the trimethylamine ethylene colactone obtained from the first stage of the multistage membrane separation system into the aqueous solution, of which the mass ratio of the trimethylamine ethylene colactone to the salt compound is or is approximate to the critical mass ratio in a liquid phase, through evaporation, crystallization, liquid-solid separation and sesalination, and returning the aqueous solution to the multistage membrane separation system so as to thoroughly separate the trimethylamine ethylene colactone and the salt compound.

Description

The method of trimethylaminyl ethlyl lactone and the multistage membrane sepn of salt compounds continous way

The present invention relates to (claim trimethyl-glycine again from betaine, glycinebetaine, Trimethyl glycine etc.) (with Mono Chloro Acetic Acid and Trimethylamine 99, perhaps Mono Chloro Acetic Acid and Trimethylamine 99 and alkali metal hydroxide, perhaps alkali-metal chloracetate and Trimethylamine 99 are raw material) (similar system comprises the aqueous solution that betaine and salt compounds for a certain reason form for the aqueous solution of chemosynthesis reaction product, the betaine and all very high aqueous solution of the two concentration of salt compounds that form of betaine and salt compounds for a certain reason particularly) isolate the method for betaine in.

Technical field

Betaine (Trimethylammonioacetate), claim trimethyl-glycine (Betaine), glycinebetaine (Glycine betaine), Trimethyl glycine (Trimethylglycine) again, U.S.'s " chemical abstracts " chemical substance index title Methanaminium 1-carboxy-N, N, N-trimethyl-, inner salt; Registration number (CAS No.) 107-43-7.Molecular formula (CH3) ₃N ⁺CH ₂COO ^-, trade(brand)name often is called BETAINE anhydrous when not containing crystal water, molecular weight 117; Trade(brand)name often is called a water trimethyl-glycine, molecular weight 135 when containing a crystal water.Nontoxic, flavor is sweet, and little have a special odor, is the minimum and amphoterics safe to eat of molecular weight.

Betaine extensively is present in animal, plant and the microbe.It is found in sugar beet juice at first, just contains this material in the beet, thus the trimethyl-glycine of gaining the name, in fact the content in the beet have only 0.1～0.3% and the level of matrimony vine similar, not as good as 0.6% of spinach.Such content causes natural betaine resource extremely limited, is difficult to satisfy the rigid demand in market.

The form of all right salt of betaine exists, and for example the hydrochloride of betaine often is called beet alkali hydrochlorate or betaine hydrochloride.Betaine hydrochloride is very strong acidity, so its use range wants much narrow compared with betaine.Betaine hydrochloride is using the chemosynthesis out-of-date methods to produce always, but owing to can't separate fully, the ubiquity product purity is low, of poor quality, yield is low, the serious problems of contaminate environment.The production of betaine hydrochloride is also because strongly-acid, thereby very high to the requirement for anticorrosion of complete production unit.

Through the development of over half a century, betaine has been a global feedstuff industry additive indispensable, safe in utilization, also is like this in China.Betaine has other materials to be difficult to the alternate critical function as fodder additives, and this is confirmed by domestic and international a large amount of scientific and technical literature data.

The metabolism of betaine and methionine(Met) has substantial connection, betaine is by providing methyl on the one hand, reduce the confession methyl consumption of methionine(Met), thereby save the intravital methionine(Met) of animal, betaine is by increasing homocysteine methyl transferase activity one by one on the other hand, promoted the conversion of homocysteine to methionine(Met), has the effect that has a net increase of methionine(Met), also play a part to save methionine(Met) in the body, the betaine that Here it is it has often been said can partly substitute the reason place of methionine(Met).The function of betaine certainly also moreover.

The interpolation betaine all has good promoter action to the growth in each stage of pig in the swine rations, and is ideal to the effect of growing swine.Betaine can promote muscle to increase and protein increases, and promotes metabolism of fat and suppresses fatty deposits, thereby significantly improve the hog on hook lean ratio, reduces the thickness of backfat.Betaine can obviously increase creatine in the fattening pig longissimus dorsi muscle, creatinine, sour insoluble carnitine and myoglobin content, improves the color of pork, thereby improves pork quality effectively.Betaine is the buffer substance of osmotic pressure violent change, can be used as the osmotic protection agent of cell.In feed, add betaine, can adapt to stress situation undertissue and body and change the heavy demand that causes owing to osmotic pressure.When grice diarrhoea causes gi tract dehydration and ionic equilibrium imbalance, betaine can prevent the cell moisture loss effectively, improve the function of Na-K pump, the hyperkalemia that prevents to suffer from diarrhoea and cause, keep and the ionic equilibrium and the micro-flora of stable gastrointestinal tract environment, probiotics is occupied an leading position, harmful bacterium can not breed in a large number, drawbacks such as the minimizing of alleviation weanling pig digestive ferment secretory volume or enzymic activity reduction, be beneficial to the secretion of endogenous digestive ferment and stablizing of the interior digestive enzyme activity of stomach and intestine, promote the g and D of duodenum fine hair, thereby improve the weanling pig digestive function, improve the digestion and the utilization of nutrient in the feed, increase food consumption, significantly reduce diarrhoea, promote that weanling pig grows fast.Because it is neutral that betaine is, and has oxidation resistant characteristic, therefore will avoid VITAMIN in adding feed, liposoluble vitamin VA particularly, VD, VE, VK is in feed processing or deposit the reduction of tiring in the process, thereby has anti-oxidation, promotes the effect of its absorption in vivo.Betaine has very positive effect to the protection of tiring of VITAMIN in Preblend.

Add betaine in the poultry diet growth fowl body fat is descended, protein content increases, and meat improves, and egg productivity increases.The effect that betaine has anti-stress and improves immunizing power can promote the growth of poultry, improves food conversion ratio.Particularly may command reduces mortality ratio because of infecting the infringement that coccidia may bring, and adds the tensile strength that betaine can improve enteron aisle, prevents to be subjected to the enteron aisle fine hair of coccidium infection chicken to reduce.We can say that anticoccidial be unable to do without betaine now.Because the application of microbiotic in feed is restricted, so the interest that people utilize betaine to improve animal intestinal health increases day by day.Betaine can reduce the risk of kind of chicken and the sex change of laying hen liver fat in addition.

The similar beneficial effect that betaine also has many fronts to narrate to aquatic animal.People are for a long time with the main feeding growth stimulant of betaine as fish, because it can improve the appetite of fish and the digestibility of nutrient thereof.Fish and crustaceans aquatic animal (as shrimp, crab etc.) are successfully being transferred to the process of sea farming from freshwater aquiculture, and betaine also plays an important role.It is that addition is big that culture fishery is made one of its characteristics of fodder additives with betaine, and demand is huge.

Culture industry except the feed that demand is huge, betaine is also used in a large number at aspects such as pharmacy industry, fermentation industry, daily-use chemical industry, health care, food-drink, farm crop, plants, and demand presents growing situation.

Betaine is a kind of lipotropic factor, can effectively prevent, reduce the accumulation of fat in the liver; Thereby reducing high serum homocysteine concentration by the methionine(Met) circulation, betaine is of value to cardiovascular health.So use betaine more and more in the food-drink now.Can imagine that along with improving constantly of human living standard, under " rich man disease " increasing situation, perhaps betaine (trimethyl-glycine) can walk close to the general population's daily life more and more.

Background technology

Chemical synthesis prepares betaine, the part of most critical is the salt compounds of separation and the association of betaine equimolar amount, this mainly is a sodium-chlor, also has a small amount of other salts, as sodium acetate, sodium chloroacetate, dichloroacetate sodium and hydroxy acid sodium etc.Betaine separates with salt compounds such as sodium-chlor, and people did the following trial:

(1) adsorption chromatography: the isolating principle of adsorption chromatography is to utilize the difference of sorbent material to the adsorptive power of separated material, allows sorbent material flow constantly absorption of each component in the phase (solvent or gas), desorption and reach the isolating method of each component.It is very weak because sodium type Zeo-karb has stronger adsorptive power to betaine to the adsorptive power of salt compounds, according to the principle of adsorption chromatography, people attempt separating sodium-chlor with sodium type resin cation (R.C.) tower from the aqueous solution of betaine chemosynthesis reaction product.Someone is called ion chromatography, is wrong in fact, because the separation that does not have between ion-exchange and different positively charged ion or the negatively charged ion takes place.This method is repeatedly practised through numerous insiders', be the method that falls flat by generally acknowledging, reason is in the aqueous solution of betaine chemosynthesis reaction product, the absolute magnitude or its concentration that are betaine all are very high, when they flow through resin tower, though resin has stronger adsorptive power to betaine, but the absolute magnitude of its absorption very low (every gram hygrometric state resin can only adsorb 10～50 milligrams of betaines usually), liquid has just begun just to have reached saturated at once in the process, and the resin that has reached saturated absorption has just been lost the ability of chromatographic separation at once, and this is an one; They are two years old, if can not utilize the stratographic principle to separate then utilize the principle of its adsorption-desorption to separate, sodium type Zeo-karb is very low again to the absolute adsorptive capacity of betaine, if add saturated resin water desorb of having adsorbed betaine, the slow industrial production of speed is beyond forbearance.Want the rapid desorb just need be by means of other solvents, as weak ammonia, resin needs again to recover adsorptive power with acid-alkali regeneration after the ammoniacal liquor desorb, throughput lowly becomes deadly defect, the future that this method is used has thoroughly been forfeited in the acute liter of cost, the wasting of resources and environmental pollution especially in scale operation, therefore never have the industrial report that successfully uses this method via chemical synthesis production high purity betaine.Certain this method is not valueless at all yet, can also use this method at a small amount of highly purified betaine of prepared in laboratory.In addition, if a water solution system is arranged, wherein the amount of betaine seldom, and the amount of sodium-chlor is very big, must reclaim betaine again from such system, this method is also useful so.

(2) alcohol extracting is followed the example of bibliographical information (as DE2300492) very early, but but be difficult to realize large-scale industrialization production: sodium chloroacetate and Trimethylamine 99 reaction obtain the mixed solution of betaine and sodium-chlor, because the solubleness of sodium-chlor in dehydrated alcohol, anhydrous methanol, dimethyl ethanol, ethylene glycol etc. is very little, and the solubleness of betaine in alcohol is bigger, therefore mixed solution can be isolated most of sodium-chlor with pure processing repeatedly, and the repeated multiple times crystallization also can access the very high betaine of purity.But, because the price of alcohol is too high, be used for large-scale industrial production this pass with high costs of just being sorry.Reason is as follows: recovery of (one) alcohol and dehydration sharply strengthen production cost.Need evaporation to reclaim behind the ethanol-extracted betaine, need redistillation to recover state owing to absorbed moisture again near absolute alcohol; (2) Chun loss sharply strengthens production cost.The alcoholic solution of betaine needs sequence of operations such as evaporation, crystallization, separation, distillation, and loss such as its loss, volatilization, still kettle relief liquor is all very big, difficult control.(3) the low production cost that sharply strengthens of the yield of high purity betaine.Sodium-chlor also has certain solubleness in absolute alcohol, the material that is extracted still more also will bring the moisture content of a great deal of, the absolute alcohol that adds has just become to contain at once has water alcohol than juicy, cause the solubleness of liquid phase chlorination sodium, sodium chloroacetate to heighten, when betaine crystallizes out with the form of a water thing from solution, salt compounds in the system is also had to separate out from liquid phase with the crystalline form owing to losing the dissolving moisture content that relies on, in this case, it will be very difficult seeking out highly purified betaine product.Just need above recrystallization twice if obtain highly purified betaine, this causes the last yield of high purity betaine low on the one hand, cause the crystalline mother solution of pending alcohol to increase greatly on the other hand, the reclaiming load of alcohol increases greatly.Obviously, the production cost of this method and quality are all made us and can not be satisfied with, so this processing method economic worth is little.

(3) the silver salt precipitator method: have bibliographical information to react the mixing solutions that obtains betaine and calcium chloride, generate precipitation with the reaction of the calcium chloride in silver carbonate and the solution at last, obtain betaine after the separation with calcium chloroacetate and Trimethylamine 99.The loss of silver salt and recovery will make that with process production cost raises greatly again, more seriously must exhaust one's ability to guarantee not residual silver in the betaine product, otherwise, betaine is come into the market and will fatal influence be arranged.Huge difficulty in industrial this method of use is conspicuous, and this method does not have practical value.

(4) ion exchange method: it is raw material with the betaine hydrochloride that report is arranged, with obtaining the betaine product behind anionite-exchange resin exchange the removing chlorion.Will consume hydrochloric acid owing to produce the betaine hydrochloride, and the resin regeneration after the ion-exchange then needs to consume a large amount of bronsted lowry acids and bases bronsted lowries, the waste of this resource itself just makes cost sharply raise.Exchange capacity is huge in fact, says the key reasons that this is avoided using ion-exchange exactly technically, uses consequently very uneconomically by force, and the insider generally acknowledges that already this method can not be used for the scale operation betaine.

(5) method that balances each other: the someone makes betaine-sodium-chlor-water three compositions system phasor, according to this phasor the betaine synthesis reaction solution is directly carried out separating of betaine and sodium-chlor then, this method practical application is infeasible at all: when also there is a large amount of salt compounds in liquid phase, can not crystallization go out the betaine of higher degree.

(6) reverse osmosis method and nano filtering process: reverse osmosis has been widely used in water softening or fresh water advanced desalination now; Nanofiltration generally is used for non-vapo(u)rability and concentrates, and for example takes off portion water from some aqueous organic organism is concentrated.Nanofiltration also is used for desalination, mainly is desalination from aqueous organic; Reverse osmosis also is used for from the aqueous organic desalination, but this service condition is few.Reverse osmosis and nanofiltration are best suited for the very low situation of processed solution salt concentration.If salt concn is very big, because the cause of osmotic pressure certainly will will have very high operating pressure, salt concn as the aqueous solution of betaine chemosynthesis reaction product, operating pressure will reach 100 more than the normal atmosphere, and this requirement to equipment will be very high.reverse osmosis can be used in nanofiltration, and separate to economy of large scale sodium-chlor from the aqueous solution of betaine chemosynthesis reaction product? answer is negated: though reverse osmosis and nanofiltration particularly nanofiltration can be used in desalination from aqueous organic, that is meant separating of the organism of molecular weight more than 500 and salt.The molecular weight of sodium-chlor is 58.5, and the molecular weight of betaine is 117, seem that the two differs one times, but absolute dispersion has only 58.5.Up to now, humanly also do not invent out two kinds of materials that a kind of reverse osmosis membrane or nanofiltration membrane can only differ molecular weight less than 60 and be separated from each other.

(7) the concentration difference dialysis under the electrodialysis control: in the patent No. is the method that proposes in the patent of invention of ZL200410103519.9.This method is intended to utilize betaine to see through the character of semi-permeable membranes migration easily in water, is suitable for scale operation.This method allows and has reached critical mass-ratio (betaine: betaine sodium-chlor 〉=3.5～3.7) and the water solution system of salt compounds are as the dense chamber system circulation of penetrating fluid at electrodialyzer, allow water as of the light chamber circulation of diffusion liquid simultaneously at electrodialyzer, in light chamber, suppress the dialysis of salt compounds with reciprocal electrodialysis effect from the dialysis of dense chamber at betaine, thereby make light chamber diffusion liquid become the highly purified betaine aqueous solution, and then realize that economy of large scale ground produces highly purified betaine.The enormous amount salt compounds is forced through ion-exchange membrane under electric field action migration owing to do not take place in this method, thereby power consumption significantly reduces, and realize that easily quantity-produced pattern, throughput depend on the size of impellent concentration difference of betaine dialysis and the area of dialyzing.

(8) intermittent type electroosmose process: the intermittent type electroosmose process can separate sodium-chlor and obtain highly purified betaine from the aqueous solution of betaine chemosynthesis reaction product, but need additional necessary condition can realize that economy of large scale ground produces, that be exactly the patent No. be the method described in the patent of invention of ZL02159258.6: water solution system or similar system to the geostationary trimethyl-glycine of volume (betaine) chemosynthesis reaction product are carried out the light chamber circulation of continual electrodialyzer in mode intermittently, simultaneously the evaporative desalination means are applied to pass through indispensably the dense chamber of electrodialyzer round-robin, liquid volume is restricted, salt concn has been subjected to the salt solution of the dense chamber of interim control ".If there are not these necessary supplementary condition, that causes the low problem of yield through the ion-exchange membrane loss easily with regard to can't resolve betaine, also can't resolve to realize that under high density sodium-chlor thoroughly separates and the problem of acquisition solid salt compounds from the aqueous solution of betaine chemosynthesis reaction product.

The patent No. is that the method described in the patent of invention of ZL02159258.6 is fit to starting on a small scale and produces highly purified betaine (trimethyl-glycine) very much, certainly, also is fit to the highly purified betaine of scale operation (trimethyl-glycine).But, owing to be mode intermittently, the light chamber of electrodialyzer salt concn is in the process that progressively reduces always, electrodialytic load also just is in the process that progressively reduces always in the one-period, this just causes in order to make electrodialyzer always be in higher efficient state, the voltage that we have to just heighten electrodialyzer work at set intervals just obtains higher throughput in the hope of obtaining higher working current.In addition, no matter be the fresh-water tank of light chamber system or the salt water tank of dense chamber system, all need more relatively container: control the concentration of dense chamber salt for stage, in one-period, need often to switch the valve that advances and go out between the salt water tank of dense chamber system; For from a last discontinuous operation cycle transition to the next discontinuous operation cycle, also need the valve that switches into and go out between the fresh-water tank of light chamber system.Voltage, these operations again and again of valve in than middle and small scale, are not the things of a difficulty by artificial execution.But if when very extensive or even super scale operation, the frequency of these operations will significantly increase, and artificial execution can be pretty troublesome and make mistakes an easily thing.Certainly, can be with these operation automations, this obviously is to need obviously to increase investment, considering need more relatively container again, therefore when particularly super this patented method of large-scale application on a large scale, investment will be bigger, and occupation area of equipment will be many, and this is its limitation place.

Obviously be under the pattern of method described in the patent of invention of ZL02159258.6 in the patent No., difficultly when implementing on a large scale realize serialization production, the voltage-regulation, the valve that also are difficult to avoid frequent switch.Therefore seeking new method overcomes existing drawback realistic meanings has just been arranged.

Electrodialysis is as a kind of membrane separation technique, developed into from desalination, sea water desaltination and the preparing salt by working up seawater that is used for brackish water at first to be used for aspects such as environment protection, foodstuffs industry and fine chemistry industry now more and more.When electrodialysis is used as separation means, the following operating method is arranged at present:

(1) intermittent type is intermittent type as shown in Figure 1 and Figure 2.This pattern of Fig. 1 is used for the desalination of seawater or salt water at first, and this pattern of Fig. 2 then is used for to specific material desalination in broad range more.Under the feature limits condition, use intermittent type pattern, the desalination in the time of can being used for chemical synthesis production high purity betaine.The patent No. that Here it is is the method described in the patent of invention of ZL02159258.6.

(2) single-stage continous way is the single-stage continous way as shown in Figure 3, Figure 4.If the desalination when the single-stage continous way is used for chemical synthesis production high purity betaine, great drawback is arranged, because certainly will requiring fresh-water tank salts contg index must hang down satisfactory degree, continuous production can outwards carry qualified material, this just makes electrodialyzer because the control of fresh water low conductivity has to work under very low current status, and the desalination ability sharply reduces.And the aqueous solution salts contg of betaine chemosynthesis reaction product is very high, and the desalination load is extremely heavy, and therefore, from the Technological Economy angle of large-scale production, the single-stage continous way can not be tolerated fully.

(3) multistage continous way is as Fig. 5.Shown in Figure 5 and also have the multistage continous way flow process of other unlisted illustrated electrodialysis, can from the aqueous solution of betaine chemosynthesis reaction product, isolate betaine, but cost will be very high, because electrodialyzer fresh-water system one side, be that sodium-chlor or betaine concentration are all very high, sodium-chlor is moved to the process of dense chamber from light chamber by ion-exchange membrane under effect of electric field, betaine also sees through the ion-exchange membrane dialysis to dense chamber from light chamber simultaneously under the concentration difference reactive force, cause the loss of betaine in the desalination material very big, have a strong impact on yield.If reclaim the strong brine that contains material, because the water of dense chamber system is the extra fresh water that adds, the load of evaporation will be especially heavy.Above-mentioned reason causes production cost sharply to raise, and will seriously undermine the large-scale production competitiveness of product in market.

The present invention proposes the method for chemosynthesis betaine and the multistage membrane sepn of salt compounds continous way under a kind of characteristic condition, this method has solved the various drawbacks that exist when above-mentioned all background technologies are applied in the desalination of chemosynthesis betaine.

Summary of the invention

The present invention defines especially: if the aqueous solution of betaine (is raw material with Mono Chloro Acetic Acid and Trimethylamine 99 and alkali metal hydroxide or alkali-metal chloracetate and Trimethylamine 99) chemosynthesis reaction product is carried out evaporation concentration, betaine and salt compounds just at a time can be simultaneously from the aqueous solution form with solid phase separate out, the mass ratio of betaine and salt compounds just is called critical mass-ratio in the liquid phase this moment, and its value is 3.5～3.7: 1.0.The solution that has reached critical mass-ratio can be that betaine and salt compounds are in the full altogether concentrated solution of selecting, it also can be the diluent that adds behind the water, whether the aqueous solution that it only characterizes betaine and salt compounds can also separate desalination by evaporative crystallization is liquid-solid, be betaine and salt compounds the aqueous solution near or when having reached critical mass-ratio, no matter it is strong solution or dilute solution, all can not isolate pure solid salt compounds by evaporation.

In the aqueous solution of betaine chemosynthesis reaction product, the mass ratio of betaine and salt compounds is approximately 2: 1, well below critical mass-ratio 3.5～3.7: 1.0, aqueous solution of this explanation betaine chemosynthesis reaction product can pass through the pure solid salt compounds of the liquid-solid separation removal of evaporative crystallization.In fact, the aqueous solution of betaine chemosynthesis reaction product is a kind of very special salt-containing solution system, when the mass ratio of wherein betaine and salt compounds during well below critical mass-ratio, the cost of the liquid-solid separation desalination of evaporative crystallization also will be well below the cost of electrodialysis separating desalination.

It is not a kind of method of economy that the direct aqueous solution with betaine chemosynthesis reaction product send electrodialytic desalting, therefore at first must carry out the liquid-solid separation desalination of evaporative crystallization to the aqueous solution of betaine chemosynthesis reaction product, the mass ratio that makes betaine and salt compounds in the liquid phase of isolating behind the solid salt compounds near or reach critical mass-ratio.Then the liquid phase after isolating the solid salt compounds is the mother liquor adding water suitable with the front steam output after the liquid-solid separation desalination of evaporative crystallization, it also can be exactly the water of condensation that evaporates previously, make its dilution and return to initial volume substantially, then the mass ratio that obtains betaine and salt compounds in the liquid phase near or reach the aqueous solution of critical mass-ratio.

The present invention defines especially: in the liquid phase mass ratio of betaine and salt compounds near or the aqueous solution that reaches critical mass-ratio (3.5～3.7) be called stoste.The acquisition of stoste has two methods: the one, the mass ratio of betaine in the liquid phase and salt compounds departed from, carries out less than the aqueous solution of critical mass-ratio evaporative crystallization is liquid-solid to separate desalination, and the suitable thin up of liquid phase obtains then; The 2nd, the mass ratio of betaine and salt compounds departs from, obtains less than replenishing betaine (trimethyl-glycine) in the aqueous solution of critical mass-ratio in liquid phase.But second method is opposite with target of the present invention, thereby be invalid method, so, must select last method for being the aqueous solution of raw material chemosynthesis betaine reaction product with Mono Chloro Acetic Acid and Trimethylamine 99 or Mono Chloro Acetic Acid and Trimethylamine 99 and alkali metal hydroxide or alkali-metal chloracetate and Trimethylamine 99.

The desalination of stoste must have the electrodialytic membranes of feature limits condition to separate by means of additional, just as the method for the present invention's introduction.

Among the present invention, stoste be sent to as shown in Figure 6, the present invention is in particular chemical synthesis production high purity betaine and the multistage film separating system of specially designed continous way.

The multistage film separating system of continous way shown in Figure 6, the membrane sepn of each grade is made up of the electrodialyzer more than 1 or 1, the size that how much depends on segregational load of electrodialyzer equipment, the relation that the two is proportionate.If many electrodialyzers can be in parallel within the corresponding levels, also can be series connection.

The light chamber of electrodialyzer at the corresponding levels and fresh-water tank at the corresponding levels constitute the circulation loop of light chamber system at the corresponding levels; The dense chamber of electrodialyzer at the corresponding levels and dense water tank at the corresponding levels constitute the circulation loop of dense chamber system at the corresponding levels.The 1st grade of the multistage film separating system of continous way as shown in Figure 6, the light chamber of the 1st grade of electrodialyzer (1) (1 left side, signal) and the 1st grade of fresh-water tank (1A) have constituted the circulation loop of the 1st grade light chamber system by pipeline; Dense chamber of the 1st grade of electrodialyzer (1) (1 right side, signal) and the 1st grade of dense water tank (1B) have constituted the circulation loop of the 1st grade dense chamber system by pipeline.

The membrane sepn of certain one-level is to realize that promptly the salt in certain one-level fresh-water tank material is constantly transferred in the material of the dense water tank of this grade by the ion-exchange membrane of this grade electrodialyzer in a steady stream in the working cell of the circulation loop formation of this grade electrodialyzer and deep or light two systems of this grade.

All of the multistage membrane sepn of continous way shown in Figure 6 light chamber systems at different levels totally constitute the fresh water flow process of the multistage membrane sepn of continous way, and all dense chamber systems at different levels totally constitute the concentrated stream journey of the multistage membrane sepn of continous way.

Light chamber system between the two-stage produces the material association: the fresh-water tank of light chamber system at the corresponding levels is accepted the light chamber material that previous stage is sent here continuously, the light chamber material that the light chamber discharging continuous partial flow of electrodialyzer at the corresponding levels goes out the light chamber material a great deal of of sending here continuously with previous stage is sent to the fresh-water tank of one-level afterwards, so reaches the balance of light chamber at the corresponding levels material.The 2nd grade of the multistage film separating system of continous way as shown in Figure 6, the 2nd grade of fresh-water tank (2A) of the light chamber system of the 2nd grade of membrane sepn accepted the 1st grade of light chamber material of sending here continuously, and the light chamber discharging of electrodialyzer at the corresponding levels then continuous partial flow goes out the fresh-water tank that is sent to 3rd level with the light chamber material of the 1st grade of light chamber material a great deal of of sending here continuously.

Dense chamber system between the two-stage also produces the material association: the dense water tank of dense chamber system at the corresponding levels is accepted the dense chamber material that the back one-level is sent here continuously, the dense chamber material that the dense chamber discharging continuous partial flow of electrodialyzer at the corresponding levels goes out the dense chamber material a great deal of of sending here continuously with the back one-level is sent to the dense water tank of previous stage, so reaches the balance of dense chamber at the corresponding levels material.The 2nd grade of the multistage film separating system of continous way as shown in Figure 6, the dense water tank of the dense chamber system of the 2nd grade of membrane sepn is accepted the dense chamber material that 3rd level is sent here continuously, and the 1st grade dense water tank is sent in the dense chamber discharging of the electrodialyzer at the corresponding levels then continuous partial flow dense chamber material that goes out the dense chamber material a great deal of of sending here continuously with 3rd level.

The progression of the multistage film separating system of continous way as shown in Figure 6 how much, depends on the size of segregational load; Under the certain situation of load, what of progression are then relevant with the desalination ability of electrodialyzers at different levels.The definite of the multistage film separating system progression of continous way can calculate by related process.

Stoste is when the multistage film separating system of continous way that is sent to as shown in Figure 6, walk to treat the desalination material with the light chamber of the multistage film separating system of present separatory continous way, (as the system of Fig. 5) pattern difference of leaking water in dense chamber, characteristic of the present invention ground is divided into two the stoste material, simultaneously, continuously, be sent to deep or light two systems of the multistage film separating system of continous way of the present invention's design respectively: the stoste material that enters the multistage film separating system fresh water of continous way flow process is that the 1st grade of fresh-water tank (1A) enters from head end, and the stoste material that enters the multistage film separating system concentrated stream of continous way journey is that the dense water tank of N level (NB) enters from end, the overall trend of two strands of materials in this system forms relative adverse current, and the overall trend of the material in deep or light two systems forms series connection respectively between at different levels; Every grade of deep or light system in inside constitutes membrane sepn circulation closed circuit working unit separately, and salt is moved to dense chamber from light chamber.

Before the specially designed multistage film separating system of the present invention was started working, (1B～NB) all reached the stoste of suspending dense water system after the nominal volume and injects to allow stoste be injected into as shown in Figure 6 the dense water tank of the 1st grade～N level of the multistage film separating system of continous way earlier; Follow to produce flow (roughly the flow with the synthesis reaction solution generation the is suitable) beginning that produces stoste under the load and provide stoste continuously to the 1st grade of fresh-water tank of multistage film separating system, after a while, treat that starting the 1st grade of electrodialyzer when the enough circulation loops of liquid volume are worked in the 1st grade of fresh-water tank starts working.Under effect of electric field, salt in the 1st grade of fresh-water tank material begins constantly to move in the stoste material of the 1st grade of dense water tank by the ion-exchange membrane of electrodialyzer, material liquid level in the dense water tank is basicly stable, and the material liquid level in the 1st grade of fresh-water tank raises gradually.

Because what light, dense water tank injected all is stoste, therefore the concentration of electrodialyzer intermediate ion exchange membrane both sides betaine is identical, can not produce obviously excessive concentration difference, thereby betaine can be ignored substantially through the amount of film migration, the amount of betaine can not lost in the fresh-water system material, and production rate is secure.

When the material liquid level in the 1st grade of fresh-water tank was about to be elevated to specified liquid level, therefore the 1st grade of electrodialyzer certain hour of having worked had had the salt of a great deal of to transfer to the 1st grade of dense water tank from the 1st grade of fresh-water tank.With the stoste that enters the 1st grade of fresh-water tank relatively, the salt concn of material decreases drastically in the 1st grade of fresh-water tank, specific conductivity decreases drastically in other words.It is initial in the 1st grade of dense water tank that what inject also is stoste, at this moment it since accepted a great deal of shift the salt of coming from the 1st grade of fresh-water tank, its salt concn has had tangible rising, in other words with the stoste of initial injection relatively, specific conductivity has had tangible rising; The amount of betaine does not have considerable change, and the amount of salt has increased, therefore in the 1st grade of dense water tank material the mass ratio of betaine and salt compounds begin to depart from, less than critical mass-ratio.

When the material liquid level in the 1st grade of fresh-water tank is elevated to specified liquid level, just distributes and enter into the 1st grade of suitable inventory of the former liquid measure of fresh-water tank and be sent to the 2nd grade of fresh-water tank from the 1st grade of light chamber of electrodialyzer effluent liquid.Like this, the material of inflow and outflow is reached balance in the 1st grade of fresh-water tank.Electrodialyzer turns round under stable working current, and its speed from light chamber transfer salt to dense chamber is certain.Flow into the salt of the 1st grade of fresh-water tank and transfer to the salt of the 1st grade of dense water tank by the 1st grade of fresh-water tank by stoste, under the certain situation of the amount of the two, the salt concn that can cause being sent to the material of the 2nd grade of fresh-water tank from the 1st grade of light chamber of electrodialyzer effluent liquid shunting can obtain steady state at a certain trim point.

The 1st grade of membrane sepn working on.

The 2nd grade of fresh-water tank accepted the material from the 1st grade of fresh-water system, starts the 2nd grade of electrodialyzer and start working when the enough circulation loop work of liquid volume wherein.Under effect of electric field, salt in the 2nd grade of fresh-water tank material begins constantly to move in the stoste material of the 2nd grade of dense water tank by the ion-exchange membrane of electrodialyzer, material liquid level in the dense water tank is basicly stable, and the material liquid level in the 2nd grade of fresh-water tank raises gradually.

Similarly, when the material liquid level in the 2nd grade of fresh-water tank was about to be elevated to specified liquid level, therefore the 2nd grade of electrodialyzer certain hour of having worked had had the salt of a great deal of to transfer to the 2nd grade of dense water tank from the 2nd grade of fresh-water tank.With the material ratio that enters the 2nd grade of fresh-water tank by the shunting of the light chamber of upper level, the salt concn of material decreases drastically again in the 2nd grade of fresh-water tank, specific conductivity decreases drastically again in other words.It is initial in the 2nd grade of dense water tank that what inject also is stoste, at this moment it since accepted a great deal of shift the salt of coming from the 2nd grade of fresh-water tank, its salt concn has had tangible rising, in other words with the stoste of initial injection relatively, specific conductivity has had tangible rising; The amount of betaine does not have considerable change, and the amount of salt has increased, therefore in the 2nd grade of dense water tank material the mass ratio of betaine and salt compounds begin to depart from, less than critical mass-ratio.Certainly, because the time of first step membrane sepn work is longer, in the 1st grade of dense water tank material of this moment the mass ratio of betaine and salt compounds depart from, bigger less than the degree of critical mass-ratio, just with the 2nd grade of dense water tank material ratio, the specific conductivity of the 1st grade of dense water tank material is higher.

When the material liquid level in the 2nd grade of fresh-water tank is elevated to specified liquid level, just distributes and enter into the 2nd grade of inventory that the fresh-water tank inventory is suitable and be sent to the 3rd level fresh-water tank by the 1st grade from the 2nd grade of light chamber of electrodialyzer effluent liquid.Like this, the material of inflow and outflow is reached balance in the 2nd grade of fresh-water tank.Electrodialyzer turns round under stable working current, and its speed from light chamber transfer salt to dense chamber remains certain.By the 1st grade of salt that flows into the salt of the 2nd grade of fresh-water tank and transfer to the 2nd grade of dense water tank by the 2nd grade of fresh-water tank, under the certain situation of the amount of the two, the salt concn that can cause being sent to the material of 3rd level fresh-water tank from the 2nd grade of light chamber of electrodialyzer effluent liquid shunting equally can obtain steady state at a certain trim point.

The 1st grade and the 2nd grade of membrane sepn are working on.

............

Similar with said process, up to the 1st grade, the 2nd grade ... N-1 level membrane sepn is working on.

The salts contg of material is relatively in the salts contg of material and initial stoste or the 1st grade of fresh-water tank in the N-1 level fresh-water tank, the decline of huge amplitude has been arranged, salt concn has been in a very low level, the specific conductivity that shows as material aqueous solution has had the decline of huge amplitude, specific conductivity to be in a very low level.Therefore, the material in the N-1 level fresh-water tank is approaching has been highly purified aqueous solutions of betaine.Though the material in the dense water tank of N-1 level has been accepted to move the salt of coming from N-1 level fresh-water tank through N-1 level electrodialyzer, compared with the rank of front, the amount of the salt of acceptance will less or have been wanted much less.Certainly, to N-1 level membrane sepn, because fresh water control, the working current of its electrodialyzer is also little a lot.So, material in the dense water tank of N-1 level is compared with stoste, though salts contg has increased, the amplitude that increases not is very big, just the mass ratio of its betaine and salt compounds depart from, low less than the degree of critical mass-ratio than the material in the dense water tank of front one-level.

N level fresh-water tank is accepted the material from N-1 level fresh-water system, starts N level electrodialyzer and start working when wherein the enough circulation loops of liquid volume are worked.Under effect of electric field, salt in the N level fresh-water tank material begins constantly to move in the stoste material of the dense water tank of N level by the ion-exchange membrane of electrodialyzer, material liquid level in the dense water tank is basicly stable, and the material liquid level in the N level fresh-water tank raises gradually.

Equally, when the material liquid level in the N level fresh-water tank was about to be elevated to specified liquid level, therefore the N level electrodialyzer certain hour of having worked had had a certain amount of salt to transfer to the dense water tank of N level from N level fresh-water tank.With the material ratio that enters N level fresh-water tank by the shunting of the light chamber of upper level, the salt concn of material has had further decline again in the N level fresh-water tank, specific conductivity has had further decline again in other words.Now, the material salt concn in the N level fresh-water tank has been in the low-level of process goal, and the aqueous solution of high purity betaine forms.Initial injection also is stoste in the dense water tank of N level, and at this moment it is owing to accepted a certain amount of salt of coming from the transfer of N level fresh-water tank, and its salt concn has had certain rising, and the stoste with initial injection compares in other words, and specific conductivity has had certain rising; The amount of betaine does not have considerable change, and the amount of salt has increased, therefore in the dense water tank material of N level the mass ratio of betaine and salt compounds begin to depart from, less than critical mass-ratio.Since with other membrane sepn of earlier stages relatively, the time of N level work is the shortest, most importantly the amount that shifts of salt is minimum, so the concentration of salt is minimum in the dense water tank material of N level, departs from, less than the degree of critical mass-ratio also minimum.Certainly, separate comparison with the previous stages electrodialytic membranes, during N level electrodialyzer membrane sepn, its working current is also minimum.

When the material liquid level in the N level fresh-water tank is elevated to specified liquid level, just distribute and entered into subsequent disposal operation that the suitable inventory of N level fresh-water tank inventory is sent to the high purity betaine aqueous solution by the N-1 level to obtain solid-state high purity betaine from the light chamber of N level electrodialyzer effluent liquid, the material of inflow and outflow is reached balance in the N level fresh-water tank.Electrodialyzer turns round under stable working current, and its speed from light chamber transfer salt to dense chamber remains certain.Flow into the salt of N level fresh-water tank and transfer to the salt of the dense water tank of N level by N level fresh-water tank by the N-1 level, under the certain situation of the amount of the two, the material salt concn that can cause being sent to the subsequent disposal operation of the high purity betaine aqueous solution from the shunting of the light chamber of N level electrodialyzer effluent liquid equally can obtain steady state at a certain trim point.Certainly, the salt concn of this trim point is very low very low, because this material that distributes from the light chamber of N level electrodialyzer effluent liquid at last is as isolating target final mean annual increment solution, its specific conductivity has obtained reducing to greatest extent at the multistage film separating system of continous way of the present invention's design, and just salt has obtained removing to greatest extent.

So far, all membrane sepn at different levels are all worked, but the amount of the salt of membrane sepn at different levels migration is not necessarily identical; Membrane sepn loads one regularly under the production task, and by the inferior membrane sepn of back level, the migration amount of salt is few more.The salt concn of the 1st grade of dense water tank material and initial stoste have relatively had huge raising, and the enrichment of salt has reached high level.In the multistage film separating system of continous way dense water tanks at different levels, the 1st grade of dense water tank material salt concn is the highest.The 1st grade of dense water tank is to the dense water tank of N level, and wherein the salt concn of material is from high to low, and from 1 grade of dense water tank of the dense water tank to the of N level, wherein the salt concn of material is the situation that is increase in other words.

After distributing and enter into the suitable inventory of N level fresh-water tank inventory and be sent to high purity betaine aqueous solution subsequent technique since the light chamber of N level electrodialyzer effluent liquid, begin successively, in succession ... N-1 level, the dense chamber of N level electrodialyzer effluent liquid distribute and enter into the suitable inventory of dense water tank inventory at the corresponding levels only and be sent to other dense water tank of previous stage, so reach the material balance of dense water systems at different levels from the 1st grade, the 2nd grade in good time; The 1st grade of dense chamber of electrodialyzer effluent liquid distribute salt concn obtained to greatest extent that enrichment promptly departs to greatest extent, less than the material of critical mass-ratio, send to the aqueous solution and merge away from the betaine chemosynthesis reaction product of critical mass-ratio, just the material that distributes of the 1st grade of dense chamber of electrodialyzer effluent liquid is got back to the technology status of the aqueous solution of betaine chemosynthesis reaction product, can be in the lump by the cheap liquid-solid separate mode desalination of evaporative crystallization.The dense water tank of N level then injects stoste continuously, certainly distribute with the 1st grade of dense chamber of electrodialyzer effluent liquid according to its flow of material balance, equate the concentrated stream amount of association between the dense water systems at different levels in the multistage membrane sepn flow process of continous way of the design of the present invention just with mass flow that the aqueous solution away from the betaine chemosynthesis reaction product of critical mass-ratio merges.

The multistage membrane sepn of the continous way of chemosynthesis betaine and salt compounds has so far just been gone on the track of normal operation: stoste is divided into two and enters the two ends of multistage film separating system in the mode of adverse current continuously respectively, from the multistage film separating system of continous way the 1st grade is that head end enters the fresh water flow process continuously, and last is that the light chamber of tail end obtains the highly purified betaine aqueous solution continuously in the light chamber of N level of the multistage film separating system of continous way; N level from the multistage film separating system of continous way is that tail end enters the concentrated stream journey continuously, last in the 1st grade of dense chamber of the multistage film separating system of continous way be the dense chamber of head end obtain continuously salt concn obtained to greatest extent that enrichment promptly departs to greatest extent, less than the dense water material of critical mass-ratio, this material is then got back to the technology status identical with the aqueous solution of betaine chemosynthesis reaction product.

The betaine that the present invention proposes and the method for the multistage membrane sepn of salt compounds continous way, must be combined with to depart to greatest extent, less than critical mass-ratio, be that the dense water material that the dense chamber of head end obtains carries out the liquid-solid separation desalination of evaporative crystallization from the 1st grade of dense chamber of the multistage film separating system of continous way.Fortunately, this technological process fully can with the aqueous solution away from the betaine chemosynthesis reaction product of critical mass-ratio is carried out liquid-solid this process of desalination of separating of evaporative crystallization and merges, thereby do not produce new, extra technological process, therefore, technological process is succinct.

Specially designed multistage film separating system is operation continuously because the present invention is in particular chemical synthesis production high purity betaine, during normal operation, the working order of electrodialyzers at different levels, the material salts contg of deep or light water systems at different levels is stable, geostationary, thereby do not need periodicity frequently to regulate the operating voltage or the electric current of electrodialyzer, there is not the periodically frequent situation of switching pipeline valve of needs yet, during extensive even ultra-large production also is like this, so the investment aspect automatic control is so big in the time of can not resembling extensive enforcement ZL02159258.6.

The overall trend of two strands of stoste materials in the multistage film separating system of continous way forms relative adverse current, the result cause from the 1st grade to the N level, the salt concn of light chamber material is from high to low, the salt concn of corresponding dense chamber material also is from high to low.The original idea of this design is that to dwindle as far as possible and stablize deep or light chambers at different levels be that salt concn between the deep or light systems at different levels material is poor, reduce the salt that produces because of the concentration difference reactive force from dense chamber to the reverse migration of light chamber, to reduce the effective consumption of electric energy in fact exactly.If the overall trend of two strands of stoste materials in the multistage film separating system of continous way, not to form relative adverse current but form totally to move towards identical and stream, so from the 1st grade to the N level, the salt concn missionary society of deep or light material is increasing, will be extremely serious to the reverse concentration diffusion of N level salt.The purpose that reduces the electric energy effective consumption like this is to be difficult to realize, thereby deep or light material totally moves towards and stream just is not economic flow and method.

The light chamber of the multistage film separating system of continous way of current trend all is simply placed in-line, the effluent liquid that is the light chamber of previous stage is all directly to be sent to the light chamber of next stage electrodialyzer, as shown in Figure 5, fresh-water tanks at different levels only play a material transition, make things convenient for power to carry.This pattern increases the progression of membrane sepn in other words greatly for the flow process that the membrane sepn of big load desalination can seriously elongate material; And can be because of the service efficiency of fresh water control reduction electrodialyzer equipment for the desalination of little load.

The present invention design be exclusively used in the at different levels dense of chemosynthesis betaine and the multistage film separating system of the isolating continous way of salt, fresh-water tank, they are not only to play the material transition, the effect that makes things convenient for power to carry, more crucial, their dense with the electrodialyzer of the corresponding levels separately of what is more important, light chamber constitutes circulation loop, by designing the residence time of each side material, can serve as the material desalination of big load or even super big load simultaneously, the membrane sepn of enrichment, by electrodialyzer device layout flexibly, allow most equipment be in very high separation efficiency state to greatest extent.

Generally all there is circulation loop the at different levels dense chamber of the multistage film separating system of continous way of current trend, but its objective is mass transfer between strengthening membrane.Dense water tank at different levels is exactly to inject fresh water originally, and acceptance can be shifted to previous stage or back one-level after moving the salt of coming from the light chamber of the corresponding levels, more be the overflow discharging, as shown in Figure 5.This is for the desalination of macromolecular substance, as the desalination of protolysate, except efflux weak brine to environment friendly inadequately less than other big problems.But this can not be used for the chemosynthesis betaine and separate with salt, and reason is that betaine is easily moved to dense chamber through ion-exchange membrane, and the betaine enormous amount in the dense water is impatient at the externally loss of discharging of dense water.

We can say that the multistage film separating system of the continous way of current trend all is a quick desalination of only pursuing light chamber liquid, all insufficient consideration makes the service efficiency maximization of electrodialysis appts.

The chemosynthesis betaine that the present invention proposes and the method for the multistage membrane sepn of salt continous way, pursue the highest service efficiency of membrane separation plant, that is: still to not pursue and make the fast as far as possible desalination of the stoste material that enters light chamber to obtain the highly purified betaine aqueous solution as early as possible, also to pursue make the fast as far as possible salt enrichment of the stoste material that enters dense chamber with obtain as early as possible to depart to greatest extent, less than the dense water material of critical mass-ratio, thereby help accelerating the liquid-solid separation desalination of evaporative crystallization.

About above explanation of the present invention, the continous way multi-stage membrane separation process of intactly having described the present invention's proposition is how to realize that chemosynthesis betaine and salt compounds are thoroughly isolating.

Some drawbacks that method of the present invention has avoided existing method to exist, but method of the present invention not too is suitable for small-scaleization production, and implementing the present invention in addition on a large scale then need be based on excellent technical capability.

Description of drawings

Fig. 1: intermittent type, 1. electrodialyzer, the 2. dense chamber of electrodialyzer, the 3. light chamber of electrodialyzer, 4. dense water tank, 5. fresh-water tank is 6. treated the desalination material, 7. desalination material, 8. strong brine material.

Identical material is intermittently injected in deep or light chamber, after desalination of light chamber or the salt enrichment realization of goal of dense chamber, externally discharges material.Be usually used in salt water or sea water desaltination or their enrichment salt manufacturing.

Fig. 2: intermittent type, 1. electrodialyzer, the 2. dense chamber of electrodialyzer, the 3. light chamber of electrodialyzer, 4. dense water tank, 5. fresh-water tank is 6. treated the desalination material, 7. fresh water, 8. desalination material, 9. strong brine.

Material inequality is intermittently injected in deep or light chamber, and general light chamber is to treat the desalination material, and dense chamber is common fresh water.Material is externally discharged after treating desalination material desalination realization of goal in light chamber.Be usually used in the desalination of saliferous materials such as foodstuffs industry, fine chemistry industry.

Fig. 3: the single-stage continous way, 1. electrodialyzer, the 2. dense chamber of electrodialyzer, the 3. light chamber of electrodialyzer, 4. dense water tank, 5. fresh-water tank is 6. treated the desalination material, 7. desalination material, 8. strong brine.

Deep or light chamber is injected identical material continuously, and the deep or light system of electrodialyzer has circulation loop respectively, draws deep or light material respectively continuously from the deep or light chamber of electrodialyzer.The seawater or the salt water salt manufacturing enrichment that can be used for low water continous way desalination of saltiness or supersalinity.

Fig. 4: the single-stage continous way, 1. electrodialyzer, the 2. dense chamber of electrodialyzer, the 3. light chamber of electrodialyzer, 4. dense water tank, 5. fresh-water tank is 6. treated the desalination material, 7. fresh water, 8. desalination material, 9. strong brine.

Deep or light chamber is injected material inequality continuously, and dense chamber generally is to inject water; The deep or light system of electrodialyzer has circulation loop respectively, draws deep or light material respectively continuously from the deep or light chamber of electrodialyzer.Be usually used in the desalination of saliferous materials such as foodstuffs industry, fine chemistry industry.

Fig. 5: multistage continous way, 1. the 1st grade of electrodialyzer, the 1st grade of fresh-water tank of 1A., 1B. the 1st grade of dense water tank, 2. the 2nd grade of electrodialyzer, the 2nd grade of fresh-water tank of 2A., 2B. the 2nd grade of dense water tank, 3. 3rd level electrodialyzer, 3A. 3rd level fresh-water tank, 3B. the dense water tank of 3rd level, N. N level electrodialyzer, NA. N level fresh-water tank, NB. the dense water tank of N level is 4. treated the desalination material, 5. fresh water, 6. desalination material, 7. overflow discharging salt solution.

Deep or light chamber is injected material inequality continuously, and dense chamber generally is to inject water; Light chambers at different levels do not have circulation loop, form simply series connection; Mass transfer is standing circulation loop in order to strengthen in dense chambers at different levels, and the fresh water of often regularly adding at different levels are also regularly discharged dense water; The light chamber of final stage obtains desalination material continuously.Be usually used in fairly large macromolecule material desalination.

Fig. 6: the multistage film separating system of the continous way of chemosynthesis betaine, 1. the 1st grade of electrodialyzer, the 1st grade of fresh-water tank of 1A., 1B. the 1st grade of dense water tank, 2. the 2nd grade of electrodialyzer, the 2nd grade of fresh-water tank of 2A., 2B. the 2nd grade of dense water tank, 3. 3rd level electrodialyzer, 3A. 3rd level fresh-water tank, 3B. the dense water tank of 3rd level, N. N level electrodialyzer, NA. N level fresh-water tank, the dense water tank of NB. N level, 4. stoste material (treating desalination), 5. the stoste salt solution material behind the enrichment, 6. stoste material (salt is treated enrichment), the 7. material of desalination stoste, 8. chemosynthesis, 9. evaporation, 10. crystallization, 11. liquid-solid separation, 12. dilution, 13. isolated solid sodium chlorides

Fig. 6 is referring to summary of the invention one joint.

Embodiment

Embodiment:

With Mono Chloro Acetic Acid, caustic soda and Trimethylamine 99 is the extensive chemosynthesis betaine of raw material, obtains the aqueous solution material of reaction product.This material output flow is 9.5M ³/ hr, wherein the content of betaine is 14.74% (W/V, the back is together), and the content of salt is 7.37%, and the mass ratio of betaine and salt is 14.74/7.37=2, is far smaller than critical mass-ratio 3.5～3.7.

According to the present invention, at first it is carried out the liquid-solid separation desalination of evaporative crystallization.Liquid-solid isolate salt 300kg/hr after, in the liquid phase mass ratio of betaine and salt be (9.5 * 14.74%)/(9.5 * 7.37%-0.300)=3.50, near or reached critical mass-ratio.

The thin up material returns to original volume and forms stoste, and promptly the stoste growing amount that is caused by chemosynthesis is 9.5M ³/ hr.The content of betaine remains 14.74% in the stoste, and the content of salt is then reduced to (9.5 * 7.37%-0.300) ÷, 9.5 * 100=4.21%.

Its flow process of multistage film separating system as shown in Figure 6.This example is established 7 grades of membrane sepn, 8 of preceding 5 grades every grade configuration electrodialyzers, 6 of back 2 grades every grade configuration electrodialyzers.Every grade configures dense water tank and fresh-water tank, corresponding pipeline, pump etc. respectively, makes them constitute circulation loop respectively with the deep or light chamber of electrodialyzer at the corresponding levels separately and realizes the overall material flow trend of relative adverse current shown in Figure 6.

Stoste is injected into all dense water tanks of 7 grades, all reaches to suspend behind the nominal volume and inject.Change the fresh-water tank that stoste is imported the 1st grade of membrane sepn, import flow yes 9.5M ³/ hr.

In case starting the 1st grade of all electrodialyzers when wherein material is enough starts working.Salt in deep or light two circulation loops operation at the corresponding levels, the 1st grade of fresh-water tank material is constantly moved in the material of the 1st grade of dense water tank by the ion-exchange membrane in the electrodialyzer.The stoste of deep or light both sides begins to change: salt begins enrichment in the stoste of dense water tank, and salt concn begins to reduce in the stoste of fresh-water tank.

After the 1st grade of fresh-water tank material flows into and reaches nominal volume, immediately from the light chamber effluent liquid of the 1st grade of electrodialyzer with 9.5M ³The 2nd grade of fresh-water tank is sent in the flow shunting of/hr, starts the 2nd grade of all electrodialyzers equally and start working when wherein inventory is enough.

The aforesaid operations of all imitating at different levels afterwards, up to the 7th grade of fresh-water tank material flow into reach nominal volume after, immediately from the light chamber effluent liquid of the 7th grade of electrodialyzer with 9.5M ³The subsequent treatment process operation of the high purity betaine aqueous solution is sent in the flow shunting of/hr.Subsequently in good time in concentrated stream journey one side, earlier since the 1st grade of dense chamber effluent liquid by the 1st grade of electrodialyzer with certain flow, this example is with 9.5M ³/ hr, the liquid-solid separation desalinating process of evaporative crystallization unit is sent in shunting, and the dense chamber effluent liquid that makes the 2nd grade of electrodialyzer then is also with 9.5M ³The 1st grade dense water tank, later equal similar operations at different levels are sent in the flow shunting of/hr.The 7th grade of dense water tank is then with 9.5M ³The flow of/hr is accepted stoste.

Betaine and the multistage film separating system of salt continous way begin to have entered production run now: the initial material that enters this system's fresh water flow process is a stoste, it enters from the head end of the multistage film separating system of continous way, has become the aqueous solution of high purity betaine when being flowed out by tail end; The initial material that enters this system's concentrated stream journey also is a stoste, and it enters from the tail end of the multistage film separating system of continous way, and flows out at head end, this moment it depart from greatly, less than critical mass-ratio.

This example deep or light material salt concn change lists at different levels:

The percentage concentration difference that can see deep or light water salt at different levels by last table is more or less the same between 4.24～5.25%, is basic identical; See also that simultaneously it is 1.75 from the come out mass ratio of back trimethyl-glycine and salt of head end that stoste enters the concentrated stream journey from end, depart from far away, less than critical mass-ratio 3.5～3.7.

Certainly, liquid-solid separation desalination of evaporative crystallization mass flow to be processed is 9.5M no longer just after this ³/ hr, but its 2 times.

Claims

1. trimethylaminyl ethlyl lactone when relating to chemical synthesis and producing trimethylaminyl ethlyl lactone and the isolating method of salt compounds, it is characterized in that: the aqueous solution of trimethylaminyl ethlyl lactone chemosynthesis reaction product or similar system must be prepared at first that the mass ratio of trimethylaminyl ethlyl lactone and salt compounds in the liquid phase reaches or near the aqueous solution (stoste) of critical mass-ratio (3.5～3.7), break it into two then, enter the two ends of multistage film separating system in the mode of continuously, totally moving towards relative adverse current respectively; Obtain the highly purified trimethylaminyl ethlyl lactone aqueous solution continuously from the terminal fresh water of multistage film separating system, and from the mass ratio that the dense water of head end of multistage film separating system obtains trimethylaminyl ethlyl lactone and salt compounds continuously depart to greatest extent, less than the trimethylaminyl ethlyl lactone aqueous solution of the high salt concentration of critical mass-ratio; The trimethylaminyl ethlyl lactone aqueous solution of the high salt concentration that obtains from the dense water of the head end of multistage film separating system must be transformed into that the mass ratio of trimethylaminyl ethlyl lactone and salt compounds the liquid phase reaches or near the aqueous solution (stoste) of critical mass-ratio (3.5～3.7) and get back to multistage film separating system.

2. method according to claim 1, the material that it is characterized in that entering multistage film separating system must be that the mass ratio of trimethylaminyl ethlyl lactone and salt compounds reaches or near the aqueous solution (stoste) of critical mass-ratio in the liquid phase, and it is to depart from far away, carry out the liquid-solid back liquid phase thin up that separates of evaporative crystallization less than the saliferous trimethylaminyl ethlyl lactone aqueous solution of critical mass-ratio and obtain by the mass ratio to trimethylaminyl ethlyl lactone in the liquid phase and salt compounds.

3. method according to claim 1, each level that it is characterized in that multistage film separating system is made up of 1 or many electrodialyzers and attached deep or light water tank thereof, the light chamber of every grade of electrodialyzer and its accessory fresh-water tank constitute light chamber liquid circulation loop at the corresponding levels, and the dense water tank of the dense chamber of every grade of electrodialyzer and its accessory constitutes dense chamber liquid circulation loop at the corresponding levels.

4. method according to claim 1, it is characterized in that: the fresh-water tanks at different levels of multistage film separating system are accepted the light chamber material that previous stage is sent here continuously, and the light chamber material that the light chamber discharging continuous partial flow of electrodialyzer at the corresponding levels goes out the light chamber material a great deal of of sending here continuously with previous stage is sent to the fresh-water tank of one-level afterwards; The at different levels dense water tank of multistage film separating system is accepted the dense chamber material that the back one-level is sent here continuously, and the dense chamber material that the dense chamber discharging continuous partial flow of electrodialyzer at the corresponding levels goes out the dense chamber material a great deal of of sending here continuously with the back one-level is sent to the dense water tank of previous stage.

5. method according to claim 1, it is characterized in that: the mass ratio of trimethylaminyl ethlyl lactone and salt compounds reaches or is divided into two near the aqueous solution (stoste) of critical mass-ratio (3.5～3.7) in the liquid phase, head end fresh-water tank that enters multistage film separating system continuously i.e. the 1st grade of fresh-water tank, and be that multistage film separating system is left as aqueous solution of ester in the high purity trimethylamine second in the light chamber of final stage electrodialyzer from the light chamber of tail end electrodialyzer; The dense water tank of tail end that enters multistage film separating system continuously is the dense water tank of final stage, and from the dense chamber of head end electrodialyzer promptly the 1st grade of dense chamber of electrodialyzer depart to greatest extent, leave multistage film separating system as the mass ratio of trimethylaminyl ethlyl lactone and salt compounds less than the trimethylaminyl ethlyl lactone aqueous solution of the high salt concentration of critical mass-ratio.

6. method according to claim 1, it is characterized in that from the dense chamber of head end electrodialyzer of multistage film separating system promptly the trimethylaminyl ethlyl lactone aqueous solution of the high salt concentration that obtains of the 1st grade of dense chamber of electrodialyzer must be during returning to liquid phase the mass ratio of trimethylaminyl ethlyl lactone and salt compounds reach or stoste status near critical mass-ratio (3.5～3.7) after return multistage film separating system.