CN102219770A - Method for manufacturing high purity sodium dehydroacetate through membrane filtration - Google Patents

Abstract

The invention discloses a method for manufacturing high purity sodium dehydroacetate through membrane filtration. The method comprises the following steps: material preparing, press filtrating, crystallizing, pumping filtrating, dehydrating, rough crushing, bake drying, discharging, crushing and packaging. The preparation method provided by the present invention is simple. Sodium dehydroacetate prepared with the method has advantages of high purity, good color, high quality, and good anticorrosion effect. The purity of the prepared sodium dehydroacetate reaches above 99.5%.

Description

A kind of membrane filtration is made the method for high purity sodium dehydroacetate

Technical field:

The present invention relates to a kind of membrane filtration and make the method for high purity sodium dehydroacetate.

Background technology:

The food preservation additive that uses in food-processing at present mostly is potassium sorbate and Sodium Benzoate, yet all there is certain limitation in the germ resistance of these sanitass, potassium sorbate is very unstable in air, excessive absorption can influence HUMAN HEALTH, and Sodium Benzoate can bring peculiar smell to food, be difficult to reach the ideal preservative effect, and existing Sodium dehydroacetate adopts the synthetic method under solid-state situation, this method synthetic Sodium dehydroacetate purity is low, and purity can only reach more than 95%, quality is unstable, color is inferior.

Summary of the invention:

The objective of the invention is in order to overcome above deficiency, provide a kind of membrane filtration to make the method for high purity sodium dehydroacetate.

Purpose of the present invention is achieved through the following technical solutions: a kind of membrane filtration is made the method for high purity sodium dehydroacetate, may further comprise the steps:

A, get the raw materials ready;

B, feed intake;

C, press filtration: will react feed liquid circulation press filtration 1.5 hours, begin to take a sample from pipeline, take a sample with beaker in the valve, there is situation in activated carbon in the observation mother liquor, observes every sampling in 10 minutes, till mechanical impurity particles such as non-activity carbon, thereby obtain the reaction feed liquid and the waste active carbon of non-activity carbon, waste active carbon is discharged reactor, and at whole pressure-filtering process, temperature in the kettle should remain on 80 ℃;

D, filtration: a film filter that adopts laminar nano pottery level film to become, the aperture of strainer is 0.00-1um, hold back the impurity in the reflection liquid, further concentrate and the purifying feed liquid in effective constituent, thereby play the effect of separation and purification material, effectively the control product purity makes the purity of product bring up to massfraction more than 99.5%;

E, crystallization;

F, suction filtration;

G, dehydration;

H, coarse crushing, oven dry, discharging;

I, packing;

The present invention compared with prior art has the following advantages:

The ceramic membrane filter device of the present invention by adopting laminar nano level film to make, the filter opening of strainer is 0.001-1um, thereby will react the impurity filtering that some are invisible to the naked eye in the feed liquid, effective constituent in the reaction feed liquid is fully held back, further concentrate and the purifying feed liquid in effective constituent, thereby play the effect of separation and purification material, purify reaction solution, effectively control product purity, make that the purity of product is more than 95% by the initial quality mark, bring up to massfraction more than 99.5%, the reaction feed liquid of producing like this meets CNS GB25547 fully, U.S. food chemical code (FCC) standard, and the favorable anti-corrosion effect of the Sodium dehydroacetate that produces.

Embodiment:

In order to deepen the understanding of the present invention, the invention will be further described below in conjunction with embodiment, and this embodiment only is used to explain the present invention, do not constitute the qualification to protection domain of the present invention.

The present invention relates to a kind of membrane filtration and make the embodiment of the method for high purity sodium dehydroacetate, may further comprise the steps:

At first prepare distilled water, dehydroacetic acid (DHA), sodium hydroxide, then distilled water is put in the reactor; Open and stir, opening steam jacket heats, when treating pot temperature rise, begin to drop into Sodium dehydroacetate, drop into sodium hydroxide again to 45-50 ℃, guarantee distilled water: dehydroacetic acid (DHA): the mass ratio of sodium hydroxide is 1～1.1:0.7～0.9:0.1～0.3, feed intake finish after, from newly opening steam valve, when temperature in the kettle rises to 77 ℃, turn down quantity of steam, make temperature-stable; Measure pH value, after pH value reaches 9, be incubated 15 minutes, begin to add gac, 80 ℃ are incubated 1 hour; To react feed liquid circulation press filtration 1.5 hours again, begin to take a sample from pipeline, take a sample with beaker in the valve, there is situation in activated carbon in the observation mother liquor, observes every sampling in 10 minutes, till mechanical impurity particles such as non-activity carbon, thereby obtain the reaction feed liquid and the waste active carbon of non-activity carbon, waste active carbon is discharged reactor, and at whole pressure-filtering process, temperature in the kettle should remain on 80 ℃; Press filtration finishes the film filter that the back adopts laminar nano pottery level film to become, the aperture of strainer is 0.00-1um, hold back the impurity in the reflection liquid, further concentrate and the purifying feed liquid in effective constituent, thereby play the effect of separation and purification material, effectively the control product purity makes the purity of product bring up to massfraction more than 99.5%; Reaction feed liquid after filtering is totally put into crystallization kettle to be stirred, carry out precooling, when temperature of charge drops to 45-50 ℃ in crystallization kettle, precooling finishes, and the cooling of beginning chuck is when temperature in the kettle drops to below 18 ℃, begin to note observing the crystallization situation, when the reaction feed liquid was thick shape, then crystallization finished, and prepares blowing; Open the crystallization kettle bottom valve, while stirring the crystallization material is put into the suction filtration pond, open vacuum pump, suct rubber bumper in the dashpot water port, check whether vacuum tightness rises, open the filter tank vacuum valve, as there being material to overflow around the pond, shovel in the mother liquor with scoop, until draining mother liquor, the mother liquor of drawing back is reentered in the reactor; Enter and dig the material and the centrifuge dewatering of packing in the suction filtration pond, the mother liquor of deviating from also is reentered in the reactor; Carry out coarse crushing, oven dry, discharging again: piece of the material after will dewatering takes out, the go-cart of packing into, in go-cart, just broken material earlier, use the stainless steel scoop then, material is shoveled in the primary crusher hopper, evenly feeding in feeding procedure, and often clear up discharge port, the material that coarse crushing is good is packed in the pallet, evenly push away flat after, the go-cart of packing into pushes in the baking oven, oven dry, temperature maintenance is 89～90 ℃ in the baking oven, drying time is 18～24 hours, behind feel feel dry materials, opens oven door, cool off half an hour with the blower fan exhausting, the beginning discharging; Pack after the discharging, earlier internal packing is carried out disinfection during packing, carry out the branch packing then;

The present invention is by adopting press filtration and filtration, the ceramic membrane filter device that adopts laminar nano level film to make, the filter opening of strainer is 0.001-1um, thereby will react the fine impurity filtering that some are invisible to the naked eye in the feed liquid, effective constituent in the reaction feed liquid is fully held back, further concentrate and the purifying feed liquid in effective constituent, thereby play the effect of separation and purification material, purify reaction solution, effectively control product purity, make that the purity of product is more than 95% by the initial quality mark, bring up to massfraction more than 99.5%, the reaction feed liquid of so producing meets CNS GB25547 fully, U.S. food chemical code (FCC) standard, the high purity that produces, the better Sodium dehydroacetate of preservative effect.

Claims (1)

1. the method for a membrane filtration manufacturing high purity sodium dehydroacetate is characterized in that, may further comprise the steps:

A, get the raw materials ready;

B, feed intake;

C, press filtration: will react feed liquid circulation press filtration 1.5 hours, begin to take a sample from pipeline, take a sample with beaker in the valve, there is situation in activated carbon in the observation mother liquor, observes every sampling in 10 minutes, till mechanical impurity particles such as non-activity carbon, thereby obtain the reaction feed liquid and the waste active carbon of non-activity carbon, waste active carbon is discharged reactor, and at whole pressure-filtering process, temperature in the kettle should remain on 80 ℃;

D, filtration: a film filter that adopts laminar nano pottery level film to become, the aperture of strainer is 0.00-1um, hold back the impurity in the reflection liquid, further concentrate and the purifying feed liquid in effective constituent, thereby play the effect of separation and purification material, effectively the control product purity makes the purity of product bring up to massfraction more than 99.5%;

E, crystallization;

F, suction filtration;

G, dehydration;

H, coarse crushing, oven dry, discharging;

I, packing.