JP2009091534A - Method for producing powdery agent - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a powdery agent, by which it becomes possible to use a process agent causing solidification and aggregation by the absorption of moisture as a bulk-increasing agent even in the case that a compound containing free water is blended. <P>SOLUTION: The method for producing the powdery agent comprises adding a compound containing free water into a mixture comprising a powdery agent exhibiting acidity and a powdery agent exhibiting alkalinity, then continuously agitating and mixing the resulting mixture until foaming and adhesiveness generated by chemical reactions between components contained in the mixture become weak, further adding a process agent into the agitated and mixed material, and further agitating and mixing the resulting mixture. Thereby, the powdery agent maintaining powdery properties and having excellent flowability and non-caking property can be obtained. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

Detailed Description of the Invention

Industrial application fields

  The present invention is prepared in a stirring and mixing apparatus by adding a compound containing free water (hereinafter referred to as B compound) to a mixture of an acidic powder agent and an alkaline powder agent (hereinafter referred to as A mixture), It is related with the manufacturing method which obtains the powder agent which maintained the property of the powder and was excellent in fluidity | liquidity and non-caking property by adding a process agent.

  Conventionally, when manufacturing a powder agent, sodium sulfate (sodium salt) has been widely used as a bulking role. However, mirabilite is so hygroscopic that it can be used as a desiccant, and when combined with a compound containing free water, it forms a hydrate and causes consolidation and aggregation. Therefore, the fluidity is poor, and a powdered product that has been caked is formed, making packing during production difficult, and further problems such as appearance problems and difficulty in accurately measuring when used.

  When a raw material containing free water is blended into a powder, a production method including steps of concentration and spray drying is mainstream, but energy consumption is large and the influence on the environment is very large. In addition, for example, a method of continuously supplying a liquid anionic surfactant acid and a granular alkali powder to obtain a granular component of the powder is also known. Zeolite such as aluminosilicate is used (Patent Document 1). Zeolite also has the effect of adsorbing moisture in the same way as mirabilite, but does not cause consolidation or agglomeration unlike mirabilite, so even if free water is added at the same time, the fluidity does not deteriorate as much as mirabilite.

However, zeolite is an insoluble compound, and when mixed with a powder agent, it causes undissolved residue, adhesion to an object to be cleaned, and the like. On the other hand, mirabilite is easily soluble, but if any moisture remains in the powder, it causes consolidation and agglomeration, so it cannot be used as a bulk increase under the same moisture conditions as zeolite.
JP 2004-176055 A JP 2003-13093 A JP 2006-70231 A

Problems to be solved by the invention

  In the present invention, even when a compound containing free water is blended, a process agent that absorbs moisture to cause consolidation and agglomeration can be used as a bulking agent, maintaining powder properties, fluidity and It aims at providing the manufacturing method of the powder agent excellent in non-caking property.

Means for solving the problem

  As a result of intensive studies, the present inventors have added B compound to A mixture, and continued stirring and mixing, resulting in a mixture obtained by weakening foaming and tackiness caused by a chemical reaction between the mixtures [below The process agent was added to the mixture, and the mixture was stirred and mixed to succeed in finding a method for producing the above-mentioned powder agent.

The invention's effect

  In the production method according to the present invention, by adding a process agent to a C mixture obtained by continuously stirring and mixing a compound containing free water with the A mixture, the binding between the process agent and moisture is prevented. A powder for the above purpose can be produced.

  Hereinafter, embodiments of the present invention will be described in detail.

  The method for producing a powder preparation of the present invention includes a step of obtaining a C mixture by adding a B compound to an A mixture and continuously stirring and mixing to obtain a C mixture (hereinafter referred to as a chemical reaction step). It is characterized by.

  In the present invention, a stirring and mixing device having a stirring blade can be used. Examples of the stirring and mixing apparatus used in the present invention include a ribbon mixer, a Redige mixer, a Nauter mixer, a Henschel mixer, and a high-speed mixer. The most suitable stirring and mixing apparatus for the present invention is mixing in a chemical reaction step. From the viewpoint of efficiency, a ribbon mixer is preferable.

  In the present invention, during the chemical reaction process, the powder appearance changes stepwise. The C mixture indicates a mixture obtained in this process at a stage where foaming due to a chemical reaction and tackiness are weakened. Details of the appearance change in the chemical reaction process will be described below.

<Details of appearance change in chemical reaction process>
By adding the B compound to the A mixture and continuing the stirring and mixing, the powdery appearance changes in five stages as follows.
[First stage]
When the A mixture and the B compound are mixed, large foaming occurs, resulting in a whip shape.
[Second stage]
Foam is settled and loosened into powder.
[Stage 3]
The powder becomes sticky and becomes a dumpling lump or paste.
[Fourth stage]
The tackiness is weakened and loosens again. The powder at this point is slightly damp.
[Fifth stage]
The powdery moisture disappears and it becomes dry.

  The step of adding the process agent is preferably the fourth step. In the fourth stage, even if stirring and mixing are continued, the mixture does not foam and become sticky, and is slightly moist. In the present invention, the mixture in this state is defined as a C mixture. In addition, even if the process agent is added in the previous stage, the properties of the powder cannot be maintained or the powder has poor fluidity. When the process agent is added in the fifth stage, the C mixture becomes familiar to the process agent. Without separation.

  In this invention, in order to speed up a chemical reaction process, the temperature in a stirring and mixing apparatus can be raised. The temperature in the stirring and mixing apparatus is preferably 40 ° C. or higher, and more preferably 60 ° C. or higher.

  In this invention, the process of grind | pulverizing the powder agent obtained from mixing of a process agent and C mixture according to target quality can be added. As an apparatus or the like used in this pulverization step, a pulverizer such as a speed mill, a power mill or a cutter mill, or a sieve can be used. However, the present invention is not limited to these as long as the step of crushing the aggregated mass is obtained.

  Examples of acidic powders include citric acid, succinic acid, tartaric acid, fumaric acid, malic acid and oxalic acid, with citric acid being particularly preferred.

  Examples of the powder agent exhibiting alkalinity include sodium carbonate, potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate and the like, and sodium hydrogen carbonate is particularly preferable.

  The mixing ratio of the powder agent exhibiting acidity and the powder agent exhibiting alkalinity in the mixture A can be determined according to the intended liquid property. Here, when the final preparation is dissolved in distilled water at an arbitrary ratio, one having a pH of less than 3.0 is acidic, one having a pH of 3.0 or more and less than 6.0 is weakly acidic, 6.0 or more and 8.0 The following is defined as neutral, 11.0 or less exceeding 8.0 and weak alkalinity, and exceeding 11.0 is defined as alkaline.

  Examples of the process agent include sodium sulfate and potassium sulfate, and sodium sulfate is particularly preferable.

  The blending amount of the A mixture is preferably 1 to 55% by weight, more preferably 10 to 30% by weight. If the blending amount of the mixture is larger than the specified range, the blending amount of mirabilite will be reduced and the powder properties cannot be maintained.

  As the B compound, nonionic surfactants, anionic surfactants, amphoteric surfactants, surfactant groups of cationic surfactants, extract extracts composed of plant extracts, animal extracts, enzyme solutions, microorganisms Examples of the fermented product group composed of the extract include, but are not limited to these as long as they contain free water.

  The B compound is preferably a sophorolipid, and can be used at a composition ratio as obtained only from the fermentation and recovery steps, and at any composition adjusted artificially.

  The blending amount of the process agent is preferably 45 to 95% by weight, and more preferably 60 to 80% by weight. Below this blending amount, even when a small amount of free water remains, consolidation and agglomeration are likely to occur, and the powder properties cannot be maintained.

  The amount of water contained in the B compound is arbitrary, but the amount of the B compound is adjusted so that the amount of water is 25% by weight or less, preferably 15% by weight or less, based on the weight of the A mixture. If this amount of water exceeds the range, the chemical reaction process requires a long time and free water tends to remain, so the process agent to be added next deprives the moisture, causing caking and agglomeration. It becomes impossible to maintain the properties.

  In this invention, the process of adding the compound which does not contain free water like surfactant, an oil agent, and a solvent after addition of a process agent can be included.

  In the present invention, in order to improve the performance of the obtained powder agent, a water softener, an antifoaming agent, a fluidity modifier, a fluorescent agent, a soil redeposition inhibitor, a polymer dispersant, an enzyme, a bleaching agent, A step of adding a bleach activator, a bleach stabilizer, a chelating agent, a fragrance, a colorant and the like can be included.

  EXAMPLES Next, although an Example and a comparative example demonstrate this invention further in full detail, this invention is not limited to the following Example.

<Example 1>
In a ribbon mixer having an effective capacity of 30 kg, citric acid and sodium hydrogen carbonate shown in Table 1 were charged and stirred for 30 seconds.

  Next, the sophorolipid was uniformly added to the whole while stirring.

  In addition, when citric acid, sodium hydrogen carbonate, and sophorolipid are continuously stirred and mixed in the ribbon mixer, a change in appearance of the powder as shown in Table 2 occurs.

  After the powder entered the fourth stage, even after stirring for 10 minutes, it was confirmed that the mixture did not return sticky and maintained the same appearance, and then 1/3 of the added amount of mirabilite AO-B was added. Then, the mixture was stirred for 1 minute, and the addition and stirring were continued in 1/3 increments.

  Next, the obtained powder was transferred to a sieve having an opening of 1 mm, the aggregates that could not be crushed by the ribbon mixer were broken, and returned to the ribbon mixer again.

  Next, the antifoaming agent was added while stirring, and then Toxeal, starch-degrading enzyme, and proteolytic enzyme were added to obtain a powder.

<Comparative Examples 1-3>
Comparative Examples 1 to 3 differ from Example 1 in the stage of adding sodium nitrate AO-B. That is, in Comparative Example 1, the powder A was obtained by adding sodium nitrate AO-B in the first stage of the chemical reaction process, in Comparative Example 2 in the second stage, and in Comparative Example 3 in the third stage. The process after the addition of mirabilite was performed in the same manner as in Example 1.

  The obtained powder agent, Example 1 and Comparative Examples 1 to 3 were evaluated.

Evaluation of powder quality

  Example 1 and Comparative Examples 1 to 3 were evaluated visually based on the evaluation criteria shown in Table 3.

Liquidity assessment

  As shown in Table 3, when 50 g of Example 1 and Comparative Examples 1 to 3 were put into a funnel having an inner diameter of a thin tube portion of 6 mm, it was evaluated whether it could pass to the bottom of the funnel.

Evaluation of caking property

  A qualitative filter paper (manufactured by ADVANTEC, No. 2, 110 mm) was used to make a box without a top of 55 mm long × 55 mm wide × 2 cm high. 24 g of Example 1 and Comparative Examples 1 to 3 were placed in this box, a 5 cm × 5 cm acrylic plate was placed on the sample, and a total of 127 g of load was applied to the entire sample. In this state, it was left under constant temperature and humidity conditions of 40 ° C. and a relative humidity of 75%. One week later, the sample is gently opened on a sieve having a mesh opening of 1 mm, sieved with an electromagnetic sieve machine (manufactured by Resh) under the conditions of a vibration scale of 1 and a vibration time of 30 seconds, and the mesh-on rate according to the following formula (1) (%) Was calculated. Evaluation was performed based on the evaluation criteria shown in Table 3.

  The evaluation results are summarized in Table 4.

  Only in Example 1, excellent evaluation results were obtained for all evaluation items. In Comparative Example 1 in which mirabilite was added to the first stage, insufficient evaluation results were obtained in all items, and in Comparative Example 2, insufficient results were obtained with respect to evaluation contents other than non-caking properties. In Comparative Example 3, no aggregate was formed and the non-caking property was excellent, but the fluidity was not excellent. That is, up to the third stage, free water remained in the powder, and it was considered that this was absorbed into the mirabilite and caused aggregate formation and poor fluidity. It was found that the remaining free water did not significantly affect the caking properties, but in order to show excellent performance in all aspects of powder quality, fluidity, and non-caking properties, the chemical reaction process was performed. It turns out that it is important to go to the fourth stage.

<Example 2>
During the chemical reaction step of Example 1 described in Table 1, the internal temperature of the ribbon mixer was set to 80 ° C., and as Example 2, the change in the appearance of the powder and the time required for the chemical reaction step were set to Example 1. And are summarized in Table 5.

  In Example 1 and Example 2, there was a large difference in the time until the chemical reaction step was completed. In the case of Example 1, it was about 70 minutes, but in Example 2, it was shortened to about 20 minutes. In this embodiment, an endothermic reaction occurs in the chemical reaction step, and the temperature of the powder becomes 10 ° C to 25 ° C. Therefore, since the internal temperature in the stirring and mixing apparatus was increased from 25 ° C. to 80 ° C., it is considered that the chemical reaction was promoted and the time until the chemical reaction step was completed was significantly shortened. Moreover, in Example 1 and Example 2, the external appearance change of the powdery substance in a chemical reaction process differed. In Example 1, the powder was once loosened in the second stage, but in Example 2, there was no such stage, and the powder was paste-like in the second stage. This is also because the chemical reaction is promoted by raising the temperature in the cabinet, and the second stage in Example 1 may be shortened in Example 2. In any case, it was found that the required time can be significantly shortened by raising the temperature in the stirring and mixing apparatus in the chemical reaction step.

  Moreover, the evaluation result of the powder quality, fluidity | liquidity, and non-caking property of Example 2 was the same as Example 1.

  From the above results, by using the method for producing a powder according to the present invention, it was possible to maintain a powder property and obtain a powder having excellent fluidity and non-caking property.

  Moreover, it is clear that not only sophorolipid but also surfactants including free water, extracts, microbial fermentation products, and the like can be added to the powder agent in the same process.

Claims (10)

  By adding a compound containing free water to a mixture of a powder agent exhibiting acidity and a powder agent exhibiting alkalinity, continuing stirring and mixing, and adding a process agent to the mixture obtained by performing a chemical reaction, A method for producing a powder agent that maintains powder properties and is excellent in fluidity and non-caking properties.   2. The method for producing a powder according to claim 1, wherein in the chemical reaction, the step agent is added to the mixture obtained by continuing stirring and mixing and weakening foaming and tackiness generated.   The powder agent according to claim 1 or 2, wherein the acidic powder agent is at least one selected from the group consisting of organic acids of citric acid, succinic acid, tartaric acid, fumaric acid, malic acid and oxalic acid. Method.   The method for producing a powder according to any one of claims 1 to 3, wherein the powder having alkalinity is at least one selected from the group consisting of sodium carbonate, potassium carbonate, sodium hydrogen carbonate, and potassium hydrogen carbonate.   The compound containing free water is a nonionic surfactant, an anionic surfactant, an amphoteric surfactant, a surfactant group of a cationic surfactant, and an extract extract group consisting of a plant extract and an animal extract, and an enzyme solution The manufacturing method of the powder agent of Claims 1-4 which is at least 1 sort (s) chosen from the fermented goods group which consists of microbial extracts.   The powder according to claim 1, wherein the fermented product is a biosurfactant, and is preferably at least one selected from the group consisting of sophorolipid, rhamnolipid, glucolipid, surfactin, mannosylmannitol lipid, and trehalose lipid. Manufacturing method.   The method for producing a powder according to claim 1, wherein the process agent is at least one selected from the group consisting of sodium sulfate and potassium sulfate.   The method for producing a powder preparation according to claim 1 or 2, wherein the mixture of the powder preparation exhibiting acidity in step 1 and the powder preparation exhibiting alkalinity is 1 to 55 wt% of the total amount.   The amount of water contained in the compound containing free water in step 1 is 25% by weight or less of the amount of the mixture of the powder having the acidity and the powder having the alkalinity. The manufacturing method of the powder agent of -8.   The manufacturing method of the powder agent of Claims 1-2 and 7-9 whose process agent of the process 2 is 45 to 95 weight% of the whole quantity.