JPS62241540A - Apparatus for producing spherical particulate by w/o type reaction - Google Patents

Abstract

PURPOSE:To obtain the titled device which permits recycling of a waste gas and prevents environmental pollution by bringing the ammonia formed by the reaction of sodium silicate and ammonium sulfate into reaction with a sulfic acid and recovering and recycling the reaction product thereof as ammonium sulfate. CONSTITUTION:An emulsion suspension is formed of an aq. sodium silicate soln., different microsubstance, surface active agent and solvent. The emulsion suspension and the aq. ammonium sulfate soln. are brought into reaction in a W/O type phase in a reaction vessel to obtain the pulverized spherical particles contg. the different microsubstance. The ammonia-contg. gas generated in this stage enters an absorption column 20 from X and reacts with the dilute sulfuric acid consisting of the sulfuric acid supplied from a pipeline 21 and the water supplied from a pipeline 22 to form the ammonium sulfate. The formed ammonium sulfate is fed into an ammonium sulfate tank 23. The aq. ammonium sulfate soln. conforming to the amt. of the loss is replenished to the tank 23. The prepd. liquid is again supplied to the reaction vessel.

Description

[Detailed description of the invention] Field of use: Unreleased E! # is a milk suspension by adding so-called microcapsules that gel in an organic solvent of water rs:ais and a surfactant, and adding an aqueous solution of a second reactant as a precipitating agent to this, In a series of devices for reacting to produce spherical fine particles that are difficult to bathe in water and separating them, the second
The present invention relates to an apparatus for recovering ammonia generated in an ammonia bath using an aqueous ammonium salt solution as a reactant.

Prior art: Technical matters forming the basis of the present invention, including the first reactant, surfactant, organic solvent, etc., are disclosed in Japanese Patent Publication No. 54-62.
It is described in Japanese Patent No. 51, and in the present invention, the heterogeneous and mercury to be contained in the spherical fine particles is not limited to pigments, but useful fine particles such as microcapsules that emit fragrance can be included. .

For example, according to Example 5 of the above publication, pigment (9 powders of mercury oxide and copper oxide mixed in a ratio of 2=3 based on heavy rutting)/
O0 g was added to the first reactant (sodium silicate) aqueous solution (5
i024mof! /l) Add 500mlIclli and stir for 10 minutes to make a homogeneous suspension. This is explained using the organic solvent of the surfactant (sorbitan monooleate) (toluene, n-hexane, cyclohexane, etc. is more preferable considering its solubility and volatility in miscellaneous water, so n-hexane will be used in the following explanation). Solution (Ig//O0gr
$ solution) 1, shake it for 5 minutes with a shaker, and
/O type milk suspension I! Annual income of &. This milk suspension was added to the second
Reactant (ammonium sulfate) water solution (1 mol/l
) Add to 41 with stirring and allow to react for 30 minutes. After the reaction, the mixture was filtered, washed with water, and dried (1/O<0>C, 24 hours) to obtain 220 g of porous spherical fine powder.

The present invention relates to an improvement of an industrial apparatus for producing a non-alpha spherical fine powder containing pigment A4, as typified by Example 1 above.

Point m while attempting to solve the problem: To specifically explain the problem, the standard industrial equipment shown in FIG. 1 will be explained.

The first reactant (sodium silicate) aqueous solution that provides the gel skeleton and the heterogeneous capsules contained therein are mixed in a mixing tank) to form a suspension. This suspension, an l# agent (hexane, etc.) transported from the storage tank 114, and a surfactant (sorbitan fatty acid ester, etc.) are mixed in the FL conversion tank (2) to form a milk suspension. , and so on. This milk suspension and an aqueous solution of ammonium sulfate were mixed in a w/O phase in a reaction tank (3), and NaZO@5is2+ (NH4)2So4-5i02
A reaction as exemplified by +2N(3-)-Na, 3+H20(I) is caused to produce spherical fine particles containing the foreign trace substance. Next, solid-liquid separator (4) (centrifuge/
Solid-liquid separation is performed using a filter pre 4-strip CNP filtration device, etc.), and after washing with a cleaning liquid (water, methyl alcohol, etc.) according to the 6 sauces, the spherical fine particles are sent to a dryer at 151 K, where high-temperature gas is circulated. , do not heat before drying. Drying 1
The gas phase separated by step c is cooled in a condenser 5a, and the condensed liquid is
It is sent to a stationary tank te+. The liquid separated in the solid-liquid-juice M device (4) is sent to the standing tank (6) together with the condensed liquid, and the engraving of Seimei M-sho (no change in content)! ! It is separated into a liquid agent @ (upper stage) and an aqueous solution field (lower layer). Solvent table (upper layer) f-1 purification equipment (e.g. distillation)
f8)'& is purified, and 7t is not purified (first
It is shown by the dotted line in the middle of Z. ), sent to storage tank 1, and emulsification tank 12.
) is reused. The solution in the bottom of the stationary tank contains 5o4-, an inorganic substance such as NH4, and methyl alcohol, and is washed with methyl alcohol. If methyl alcohol is contained, fractional distillation is performed in the distillation column (7) to distill the methyl alcohol from the top of the column and send it to a storage tank for reuse. Loss methyla/L/
Replenish the new methyl alcohol entering from the CO/L/IF pipe (9). The bottom liquid of the distillation column (7) is 1,
Eliminate Qin if there is no particular need.

Ammonia is mainly generated from the reaction tank (3), part of the liquid separation tank 14), etc., and if the gas is directly released into the casing, it becomes a source of pollution, so the ammonia must be removed.

Solution: Figure 1 ) is shown in detail in Figure 2. Also, the emulsification tank 9 shown by the dotted line in FIG. 2 corresponds to the emulsification tank 2 in FIG. 1. ). The gas containing ammonia enters the absorption tower from X and reacts with dilute sulfuric acid made from sulfuric acid supplied from the pipe and water supplied from the pipe to produce ammonium sulfate. The produced ammonium sulfate is sent to an ammonium sulfate tank. The tank (c) is replenished with ammonium sulfate solution corresponding to the amount of loss and the concentration is adjusted. (&) is supplied to the reaction tank (3) in Figure 1.The nitrogen holder is a nitrogen holder, in which the gaseous portion in the system becomes substantially nitrogen, and the solvent It is used to maintain a slightly pressurized state to eliminate the risk of combustion or explosion.

Action: In the reaction tank (31), the chemical formula (D vc eriammonia?
It is generated and causes pollution, but it can be recovered by washing with sulfuric acid.

Young fruits of invention: The present invention has the following effects.

(b) Ammonia can be recovered and reused.

(b) Pollution caused by ammonia can be prevented.

[Brief explanation of drawings]

FIG. 1 is a general flow diagram of an apparatus embodying the invention. FIG. 2 shows a detailed flowchart of the flowchart of FIG. 1, particularly for ammonia recovery and production of ammonium sulfate aqueous solution. +()...Mixed species, ;2)...Emulsification tank, (3)...
Reaction tank, 14)...Solid-liquid content p! U device, ;6;...
Dryer, (6)...Stationing tank, (7)...Distillation column%1
21...Absorption tower, absorber...Ammonium sulfate tank. Applicant Sasakura Machine Manufacturing Co., Ltd. New Procedures Amendment (A) Issued in May 1986 / Date Mr. Michibe Uga, Commissioner of the Japan Patent Office ・-Indication of the case Patent application 1987-θ et al. Title of invention W / Person who corrects spherical fine particle production equipment by O-type reaction 11+1!,) 1 person in charge Patent applicant 11, A□
, 6-7-5 Goheijima, Nishiyodoyo-ku, Osaka City Name
Managing Director, Sasakura Machinery Co., Ltd. Person Date: Showa Year Month/Day Subject of voluntary amendment Specification, Detailed Description of the Invention Column 1, Page 5 of the Specification, Line 14 “Partially recycled liquid separation tank (4)” The statement has been corrected to [partial solid-liquid separation (4)]. 2. From page 5, line 19 to line 20 of the specification, "Fig. 1-1111 converged pipe section" [Fig. 4) and the pipe section where the gas pipes discharged from the gas phase section of the condenser for a methyl alcohol still distiller join together.'' Procedural amendment (method) % formula % Indication of the case Special II 1984-845956 Invention name
w7o tjIJ Reaction-based Personnel Who Corrects Spherical Fine Particle Production Apparatus 1'l Relationship Patent Applicant Address (Residence) 6-7-5-8 Gohei Wh, Nishiyodo-ku, Osaka City
(Name abbreviation) Sasakura Machinery Co., Ltd. f'? 'Shirodai
Address: 653B 4-21-9 Gamo, Higashi-ku, Osaka City
Date of order to amend the item: June 4, 1986 Target of amendment
Contents of the amendment on page 5 of the specification Attached to the application first; is an engraving of Book 1e.

Claims (1)

[Claims] 1 A dispersion is prepared by dispersing an aqueous solution of sodium silicate, which is a gelstone donor, and a foreign trace substance in a solvent that contains sorbitan fatty acid ester as a surfactant and is poorly soluble in water. ; The dispersion is reacted with an aqueous solution of ammonium sulfate as a precipitating agent to produce spherical fine particles containing the foreign trace substance; In a series of devices for separating and collecting spherical fine particles: By reaction between sodium silicate and ammonium sulfate. A device for producing spherical fine particles using a W/O type reaction, characterized in that ammonia produced is reacted with sulfuric acid and recovered and reused as ammonium sulfate.