JPH02212454A - Production of powder potassium sorbate - Google Patents

Abstract

PURPOSE:To obtain stable powdery potassium sorbate having high bulk density and free from fluidity problem by crushing and granulating dried granular potassium sorbate, etc., with a crusher or pulverizer furnished with a screen. CONSTITUTION:The objective compound can be produced in nearly 100% yield without generating off-grade by sufficiently drying granular potassium sorbate and produced by extrusion granulation, etc., separating or without separating a part or total of the granular potassium sorbate and crushing or crushing and granulating the generated off-grade such as blocks or broken fragments with a crusher or pulverizer furnished with a screen having a proper mesh opening. Potassium sorbate has mildew-proofing action and low toxicity and is useful as a preservative and mildew-proofing agent for food, etc.

Description

Detailed Description of the Invention (Industrial Application Field) The present invention relates to a method for producing powdered potassium sorbate by crushing and granulating powdered potassium sorbate using a new crusher or pulverizer. be.

[Conventional technology]

As is well known, potassium sorbate has an anti-cicada effect.
Due to its low toxicity, it has been widely used as a food preservative or anti-mold agent in recent years. Potassium sorbate manufacturers produce two types of potassium sorbate depending on their shape: granular potassium sorbate and powdered potassium sorbate. are usually manufactured.

Granular potassium sorbate is produced through a process of extrusion and granulation using a screen or die, usually around 1 MJI in diameter, a drying process, and a sieve to sort the particles that have become coarse due to multiple adhesion or are damaged. Manufactured through a process. Out-of-grade products are sent to extrusion granulation again.

On the other hand, the production of powdered potassium sorbate generally involves neutralizing potassium hydroxide and sorbic acid in an organic solvent such as acetone, methanol, or inglobanol, and then filtering and drying the crystals precipitated by the neutralization reaction. There is also a method of manufacturing through a granulation process by sieving (hereinafter referred to as "crystallization method"), or a method of manufacturing through a granulation and drying process by spraying a 40 to 60% potassium sorbate aqueous solution with a spray dryer, and a sieve separation process. This is carried out by a method of manufacturing through a sizing process using K (hereinafter referred to as the "spraying method").

(Problem to be solved by the invention) However, powdered potassium sorbate has a particle size distribution of 2>1.
Since it is a fine powder with a 50% or more mesh pass portion, when manufactured by the spray method, the powder tends to be scattered by the wind when spraying or moving the powder, so it must be collected and recycled. It is difficult to control the particle size distribution during manufacturing, and some lumps often occur, so sieving is necessary. There is a problem in that so-called out-of-grade products are generated and must be recycled. There was a problem in that it required a considerable amount of cost. In addition, powdered potassium sorbate produced by the spraying method is generally porous and has a low bulk density, so when filling and storing it in a container, it is difficult to store it unless it is submerged by shaking, which may cause problems for the end user. When handling, there were also problems such as a large amount of powder.

On the other hand, powdered potassium sorbate produced by the crystallization method is
The crystals themselves are thin scales and have very poor fluidity, so when removing powdered potassium sorbate from a packaging container, it is difficult to remove and handle, and powdered potassium sorbate and other organic acids and organic acid salts , inorganic acid salts, and other various additives (hereinafter referred to as "additives"), some users have found that it is extremely difficult to mix the mixture. was requested. Even with this method, it is difficult to control the particle size during production, and lumps are often generated, so it must be handled by sieving.
Problems arose with playback.

Furthermore, when producing granular potassium sorbate, sieving is required in the same manner as when producing powdered potassium sorbate, and there are problems associated with the production of inferior products.

[Rounding Means to Solve the Problem] As a result of intensive research to solve the various problems mentioned above, the present inventor has discovered a solution obtained through granular potassium sorbate production processes such as extrusion granulation and drying. The purpose is achieved by a new method for producing powdered potassium sorbate, in which the raw material is crushed and granulated using a crusher or pulverizer equipped with a screen, with or without separating part or all of the granular potassium sorbate. This has been achieved and the present invention has been completed.

In addition, the bulk density of the compressor and receiver increases during extrusion granulation, etc., and there is almost no problem of fine powder scattering when drying, which is the case when producing powdered potassium sorbate. The problem of fine powder scattering can be solved. 7) Separate some or all of the granular potassium undrubate and remove any lumps or small broken pieces that are not separated, either singly or in a mixture, to achieve the desired particle size distribution. By crushing or pulverizing granulation using a screen with such openings, powdered potassium sorbate can be easily produced at a yield of almost 100% without producing inferior products.

The manufacturing method of the present invention will be explained in detail below.

"Effect of Humidity" Potassium sorbate is inherently highly absorbent, and during manufacturing, it absorbs moisture from the air, causing screen clogging, and the quality of the powdered potassium sorbate produced For example, since fluidity and purity are often adversely affected, it is preferable to maintain the humidity (relative humidity) at the manufacturing site, silo, and packing area at 45% or less.

"Raw material potassium sorbate" The granular potassium sorbate used in the present invention is sufficiently dried with a water content of 0.15% or less,
Consideration will be given to making it possible to commercialize it as is. Moisture is 0.2%
If the above-mentioned raw materials are used, it is not preferable because it will be necessary to dry the produced powdered potassium sorbate. There are no particular restrictions on the particle size or shape of the granular potassium sorbate as a raw material, so it may be produced as a granular potassium sorbate with a particle size of around iff, or a lump of 20 to 30 fl with multiple pieces attached at that time. You can optionally use broken items or other non-standard items.

"Crushing granulator or crushing granulator" A crushing or crushing granulator consists of a supply port for granulated potassium sorbate, a crushing blade or a crushing blade (hereinafter referred to as a ``grinding blade, etc.''), a screen, a crushing blade, etc. A device is selected that is equipped with a motor to drive the grinder, and the powder that has been ground by the rotation of a grinding blade or the like is discharged through a screen.

Particularly preferred is a type of crusher or crusher equipped with a cage-type screen. This type of model is a soft grinding type model that grinds between a grinding blade or the like and a screen, and is suitable because the screen has a large area, allows for a large production volume, and is difficult to over-grind. The material of the powder-contacting part of the crushing or crushing granulator is preferably stainless steel, which has good abrasion resistance, and aluminum or iron is not preferable because it wears out and causes foreign matter to be mixed in. The rotation speed of the crushing blade etc. varies slightly depending on the shape and number of blades, but generally it is 1ooo to 4000.
It is about rpm.

"Adjustment of particle size" The particle size of powdered potassium sorbate can be adjusted by attaching a screen with an appropriate opening to the crusher or crusher.

For example, when manufacturing a powder with a particle size distribution such that the entire amount passes through a 32-mesh sieve and 50% or more passes through a 100-mesh sieve, the pore size is 0.4 to 0.5.
If a 111 screen is attached and manufactured, the purpose can be easily achieved. In addition, when manufacturing fine powder with a 300 mesh pass of 95% or more, 110 to 15
It can be easily manufactured by attaching a 0 mesh screen.

(Example) Examples are shown below, but the present invention is not limited to these. In addition, in the following examples, "%" means X amount %.
represents.

Example 1 A 100.3# pellet (containing 8.4 tons of water) obtained through an extrusion granulator with a screen hole diameter of 1 fin was charged into a fluidized fluid dryer equipped with a cyclone and a bag filter, and heated at 110°C.
Coarse granular potassium sorbate 96 containing lumps and powdered material with a moisture content of 0.04% after drying with hot air for 30 minutes.
．． 7 images (yield 99.8%) were obtained.

This coarse granular potassium sorbate was separated into coarse particles and fine particles using a sieve equipped with a 28-mesh wire mesh and an io mesh. ) was obtained.

The 10-mesh unit and 28-mesh unit separated by the sieve were crushed using a granulator (Kaida Seiko ■, New Speed Mill ND-30 (trademark), screen pore size 0.4ff,
The powdered potassium sorbate containing 0.04% water was crushed by supplying it to a crushing blade (rotation speed 300 rpm) at a rate of IO1/min (yield 3.4
%) was obtained. The total yield of potassium sorbate granules and powder is 99.8%. When the particle size distribution of this powdered potassium sorbate was measured, it was found that 42 mesh units were 2%, 10
0 mesh pass was 70%. In addition, using a container cut at the 200 ml position in a 500.l graduated cylinder, the bulk density was measured by dropping the container from a position 30 fl from the top of the container, and found that the bulk density was 0.44.

Example 2 20.5 kqf of extruded granulated flakes were fluidized and dried under the same conditions as in Example 1, and then the entire amount was poured into a screen with a pore size o,
Kaida Seiko New Speed Mill ND-3 with sM6 installed
0 (trademark) at a rate of 121/rnin, and water content is 0.
．． Powdered potassium sorbate 19.5% was obtained, with a bulk density of 0.45% and a particle size distribution of 42 mesh pass 4% and 100 mesh pass 66%.

This powdered potassium sorbate5. Okq and purity 9
After mixing 8.8 # of sorbic acid with a particle size distribution of 9.8%, 1% of 42 mesh mass, and 55% of 100 mesh mass in a ribbon blender for 10 minutes, the mixture was divided into 10 equal parts and the mixed state was analyzed. The concentration of is 56.7%±
It was 0.2% (risk rate 5%) and was almost uniformly mixed.

In addition, 5 kg of this powdered potassium sorbate and purity 9
After mixing 8.0 kq of fumaric acid with a particle size distribution of 9.9%, 1% of 42 mesh, and 52% of 100 mesh for 15 minutes in a ribbon blender, the mixture was divided into 10 equal parts and the concentration of 7 malic acid was analyzed. 37.5±0.3% (risk rate 5%) was almost uniformly mixed.90 Example 3 Flakes dried under the same conditions as Example 1.5. Okgt,
A 120-mesh screen was attached to the same grinder as in Example 1, and the powder was fed at a rate of 0.51/min to be ground to obtain a 300-mesh bath of 97% fine powder potassium sorbate5. Got okq.

This fine powder is 2 to 9 and the particle size distribution is 300 mesh bath 78
As a result of mixing white carbon for 8 and 9elO minutes, the potassium sorbate concentration was 20.0±0.2% (risk rate 5%), and the mixture was almost uniform.

Comparative Example 1 The bulk density of powdered potassium sorbate produced by the spray method and having a particle size distribution of 4% for 42 meshes and 64% for 100 meshes after separating particles larger than 32 meshes was measured in the same manner as in Example 1. The result was 0.33, which was small.

Comparative Example 2 The bulk density of powdered potassium sorbate produced by a crystallization method using acetone and having a particle size distribution of 1% of 42 mesh and 74% of 100 mesh after separating particles larger than 32 mesh was determined. When measured using the same method as in Example 1, it was 0.27, which was even smaller.

This powdered potassium sorbate was mixed with sorbic acid in the same manner as in Example 2, and when the mixed state was analyzed, sorbin**i was 56.7 ± 7.2% (risk rate 5%),
Uniform dispersion was not achieved. Therefore, as a result of continuing mixing for another 20 minutes, the concentration of nruvic acid was 56.7±0.
The result was 4% (risk rate 5%), and almost uniform mixing in #1 was achieved.

Next, fumaric acid was mixed in the same manner as in Example 2, but uniform mixing was difficult even after 30 minutes of mixing, and the fumaric acid concentration was analyzed to be 37.4±848% (risk rate 5%).

% compared to conventional products when mixing with acids such as Shun, salts such as phosphates and acetates, and other various additives to produce a "mixture"! -It becomes much easier. In addition, even when vibrations are applied, the bulk density is close to that of various additives, so there is less classification compared to conventional products, and it is stable enough that there is no equivalent problem in practical use.

The method of producing powdered potassium rumrubate gold by pulverizing or pulverizing eliminates the need for the expense of recovering and recycling out-of-grade products such as fine powder scattering and sieve material, which were generated in the conventional method. When producing granules, the drying process, the transport process from drying to the dry product silo, and the sieving process can produce two brands of granules and powder in one series, so there is less capital investment and less operational management. It also becomes easier.

In addition, the obtained powdered potassium sorbate has a larger bulk density than those produced by conventional methods, and has good fluidity to the extent that there is no problem in practical use.

Claims (1)

[Claims] (1) Part or all of the granular potassium sorbate is separated from the extrusion granulated and dried potassium sorbate, or the granulated potassium sorbate is not separated, and is crushed and granulated using a crusher or a crusher equipped with a screen. A method for producing powdered potassium sorbate.