CN106509368B - A kind of preparation method of feed pellet type sodium butyrate - Google Patents

Abstract

The present invention provides a kind of preparation methods of feed pellet type sodium butyrate, this method is sodium hydrate solid to be added portionwise in butyric acid and water to react, being cooled to system material after reaction becomes solid-state, solid material is directly pelletized again, target product most can be obtained through fluidized bed drying afterwards.This method does not need in the stage of reaction or a small amount of steam is only needed to heat, and is reacted using solid sodium hydroxide, and the dosage of water in reaction is greatly reduced, while reducing subsequent required dry water, reduces energy consumption；In addition, so that it can be precipitated to form solid at relatively high temperatures, consequently facilitating directly pelletizing, improving product density due to the concentration for improving product in reaction solution, avoiding dust from flying；Using fluidized bed etc., efficiently drying equipment is dried simultaneously, further decreases the energy consumption of product.

Description

A kind of preparation method of feed pellet type sodium butyrate

Technical field

The invention belongs to technical field of organic synthesis, and in particular to a kind of preparation method of feed pellet type sodium butyrate.

Background technique

Short chain fatty acids are the energy of enterocyte preference, and easily absorb out of enteric cavity, predominantly butyric acid, acetic acid and third Acid provides up to 30% maintenance energy for animal.Experiments have shown that colon blood flow can be fast after intestines intra-bladder instillation short chain fatty acids Speed increases, and disclosing it plays the role of expanding Colic vessels, and the ability of butyric acid expansion Colic vessels is strongest, and butyric acid can Inhibit the pathogenic microorganisms such as Salmonella, Escherichia coli and clostridium, increasing Bacillus acidi lactici and streptococcus fecalis etc. has Beneficial microorganism quantity has certain bacteriostasis, but since butyric acid has strong stink, and has volatility and dissociate Property, if directly applying among feed, adverse effect is easily caused, thus be usually made into relatively in herding and Feed Manufacturing Stable sodium salt.

Currently, common sodium butyrate manufacturing process be all by butyric acid aqueous solution and sodium hydroxide solution (content about 20~ 30%) it is mixed, is heated to 90~100 DEG C, reacted certain time, then reaction solution is spray-dried, obtain powder The sodium butyrate product of shape.Although the technique is simple, needs to expend a large amount of energy, such as need to heat in the stage of reaction, spraying Mist drying stage heat utilization rate is low, both increases the cost of product.In addition, the sodium butyrate product that spray drying obtains, particle It is very tiny, 120~180 mesh are generally reached, cause small product size big, specific surface area obviously increases, and is easier to the moisture absorption.

Summary of the invention

The object of the present invention is to provide a kind of preparation methods of feed pellet type sodium butyrate, can be substantially reduced energy consumption, And granular pattern product can be directly obtained.

The technical solution of the present invention is to provide a kind of preparation methods of feed pellet type sodium butyrate, including walk as follows It is rapid:

1) butyric acid and water are added into the reaction kettle with insulating layer, stirs evenly.

2) sodium hydrate solid is added into reaction kettle, sodium hydrate solid is reacted with butyric acid mixing.

3) reaction solution taking-up after reaction, is cooled to reaction solution and becomes solid-state completely.

4) spheric granules is made in the solid material for obtaining step 3).

5) the spheric granules material for obtaining step 4), which is sent into fluidized bed, dries to get granular pattern sodium butyrate is arrived.

Further, above-mentioned steps 1) in the mass ratio of butyric acid and water be 1.3~1.9:1.

Further, above-mentioned steps 2) in the ratio between the amount of substance of sodium hydrate solid and butyric acid be 1.02~1.00:1.

Further, above-mentioned steps 2) in sodium hydrate solid feed several times, and charging rate is first quick and back slow.

Further, above-mentioned steps 2) in be added sodium hydrate solid when control temperature of reaction kettle be 80~120 DEG C.

Further, above-mentioned steps 2) in sodium hydrate solid charging after reacted under 100~120 DEG C of reaction temperatures 0.5~1h.

Further, above-mentioned steps 3) in reaction solution be cooled to 70~95 DEG C.

Further, above-mentioned steps 5) in fluidized bed drying process, front half section drying temperature is controlled at 80~90 DEG C, later half Section drying temperature control is at 110~120 DEG C.

Compared with prior art, beneficial effects of the present invention:

(1) preparation method of this feed pellet type sodium butyrate provided by the invention is not needed in the stage of reaction or is only needed It wants a small amount of steam to heat, and is reacted using solid sodium hydroxide, the dosage of water in reaction is greatly reduced, reduces subsequent institute The water that need to be dried, reduces energy consumption.

(2) preparation method of this feed pellet type sodium butyrate provided by the invention is due to improving product in reaction solution Concentration consequently facilitating directly pelletizing, form granular pattern product, mention so that it can be precipitated to form solid at relatively high temperatures High product density, avoids dust from flying；Using fluidized bed etc., efficiently drying equipment is dried simultaneously, further decreases product Energy consumption.

Specific embodiment

The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel all other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.

Embodiment 1:

The preparation method for present embodiments providing a kind of feed pellet type sodium butyrate, specifically comprises the following steps:

(1) butyric acid 400kg and water 210kg is added into the reaction kettle with insulating layer, stirs evenly.

(2) it puts into sodium hydrate solid 182kg in batches into reaction kettle, according to charging rate, controls and reacted in reaction kettle Temperature is 105~110 DEG C；At the end of charging, continue that reaction temperature is kept to react 0.5h within the scope of 105~110 DEG C.

Wherein, it is preferably fed during the charging of sodium hydroxide using automatic conveying device, and charging rate early period Comparatively fast, the later period is slower；In addition, reaction temperature is excessively high can be passed through less into the collet of reaction kettle in the charging process of sodium hydroxide Cooling water is measured to reduce reaction temperature.

(3) reaction solution in step (2) reaction kettle is put into storage tank while hot, when feed liquid temperature is reduced to 95 DEG C, completely Become solid-state.

(4) spheric granules is made by oscillating granulator and spheronizator in the solid material in step (3).

(5) spheric granules material is sent into drying in fluidized bed, wherein the front half section drying temperature of fluidized bed is controlled 80 ~90 DEG C, second half section drying temperature is controlled at 110~120 DEG C, is obtained granular pattern sodium butyrate product 493kg, is detected through HPLC, should Product butyric acid sodium content is 99.82%, and being computed yield is 98.42%.

Embodiment 2:

The preparation method for present embodiments providing a kind of feed pellet type sodium butyrate, specifically comprises the following steps:

(1) butyric acid 400kg and water 300kg is added into the reaction kettle with insulating layer, stirs evenly.

(2) it puts into sodium hydrate solid 185kg in batches into reaction kettle, according to charging rate, controls and reacted in reaction kettle Temperature is 85~90 DEG C；At the end of charging, a small amount of steam is passed through to keep reaction temperature to react 1h within the scope of 100~105 DEG C.

Wherein, it is preferably fed during the charging of sodium hydroxide using automatic conveying device, and charging rate early period Comparatively fast, the later period is slower；In addition, reaction temperature is excessively high can be passed through less into the collet of reaction kettle in the charging process of sodium hydroxide Cooling water is measured to reduce reaction temperature.

(3) reaction solution in step (2) reaction kettle is put into storage tank while hot, when feed liquid temperature is reduced to 70 DEG C, completely Become solid-state.

(4) spheric granules is made by oscillating granulator and spheronizator in the solid material in step (3).

(5) spheric granules material is sent into drying in fluidized bed, wherein the front half section drying temperature of fluidized bed is controlled 80 ~90 DEG C, second half section drying temperature is controlled at 110~120 DEG C, is obtained granular pattern sodium butyrate product 495kg, is detected through HPLC, should Product butyric acid sodium content is 99.45%, and being computed yield is 98.45%.

Embodiment 3:

The preparation method for present embodiments providing a kind of feed pellet type sodium butyrate, specifically comprises the following steps:

(1) butyric acid 400kg and water 250kg is added into the reaction kettle with insulating layer, stirs evenly.

(2) it puts into sodium hydrate solid 183kg in batches into reaction kettle, according to charging rate, controls and reacted in reaction kettle Temperature is 95~100 DEG C；At the end of charging, continue that reaction temperature is kept to react 0.5h within the scope of 105~110 DEG C.

Wherein, it is preferably fed during the charging of sodium hydroxide using automatic conveying device, and charging rate early period Comparatively fast, the later period is slower, controls reaction temperature by charging rate.

(3) reaction solution in step (2) reaction kettle is put into storage tank while hot, when feed liquid temperature is reduced to 80 DEG C, completely Become solid-state.

(4) spheric granules is made by oscillating granulator and spheronizator in the solid material in step (3).

(5) spheric granules material is sent into drying in fluidized bed, wherein the front half section drying temperature of fluidized bed is controlled 80 ~90 DEG C, second half section drying temperature is controlled at 110~120 DEG C, is obtained granular pattern sodium butyrate product 498kg, is detected through HPLC, should Product butyric acid sodium content is 99.58%, and being computed yield is 99.18%.

In conclusion the preparation method of this feed pellet type sodium butyrate provided by the invention is not needed in the stage of reaction Or only need a small amount of steam to heat, and react using solid sodium hydroxide, the dosage of water in reaction is greatly reduced, subtracts simultaneously Lack subsequent required dry water, reduces energy consumption；In addition, due to the concentration for improving product in reaction solution so that its It can be precipitated to form solid under higher temperature, consequently facilitating directly pelletizing, improve product density, avoid dust from flying；It adopts simultaneously With fluidized bed etc., efficiently drying equipment is dried, and further decreases the energy consumption of product.

The foregoing examples are only illustrative of the present invention, does not constitute the limitation to protection scope of the present invention, all It is within being all belonged to the scope of protection of the present invention with the same or similar design of the present invention.

Claims (2)

1. a kind of preparation method of feed pellet type sodium butyrate, characterized by the following steps:

1) butyric acid and water are added into the reaction kettle with insulating layer, stirs evenly, the mass ratio of butyric acid and water is 1.9:1；

2) sodium hydrate solid is added into reaction kettle, sodium hydrate solid is reacted with butyric acid mixing；Wherein, sodium hydroxide The ratio between amount of substance of solid and butyric acid is 1.02~1.00:1, and sodium hydrate solid feeds several times, and charging rate is first fast Slow afterwards, control temperature of reaction kettle is 80~120 DEG C when sodium hydrate solid is added, 100 after sodium hydrate solid charging 0.5~1h is reacted under~120 DEG C of reaction temperatures；

3) reaction solution taking-up after reaction, is cooled to 70~95 DEG C, reaction solution is made to become solid-state completely；

4) spheric granules is made in the solid material for obtaining step 3)；

5) the spheric granules material for obtaining step 4), which is sent into fluidized bed, dries to get granular pattern sodium butyrate is arrived.

2. the preparation method of feed pellet type sodium butyrate as described in claim 1, it is characterised in that: the step 5) fluidisation In bed drying process, at 80~90 DEG C, second half section drying temperature is controlled at 110~120 DEG C the control of front half section drying temperature.