JP2020100809A - Method for producing fatty acid neutralization product - Google Patents

Method for producing fatty acid neutralization product Download PDF

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JP2020100809A
JP2020100809A JP2019211582A JP2019211582A JP2020100809A JP 2020100809 A JP2020100809 A JP 2020100809A JP 2019211582 A JP2019211582 A JP 2019211582A JP 2019211582 A JP2019211582 A JP 2019211582A JP 2020100809 A JP2020100809 A JP 2020100809A
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aqueous solution
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敬文 木下
Takafumi Kinoshita
敬文 木下
道哉 高木
Michiya Takagi
道哉 高木
大樹 平林
Hiroki Hirabayashi
大樹 平林
公一 福田
Koichi Fukuda
公一 福田
慶 畑
Kei Hata
慶 畑
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Kao Corp
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40Mixing liquids with liquids; Emulsifying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20Jet mixers, i.e. mixers using high-speed fluid streams
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    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/04Carboxylic acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00Making of soap or soap solutions in general; Apparatus therefor

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Abstract

To provide a method for producing a fatty acid neutralization product that can prevent formation of gel of a fatty acid neutralization product and its aggregate.SOLUTION: This method for producing a fatty acid neutralization product includes a mixing step in which a fatty acid blend liquid A is mixed with a basic aqueous solution B. The fatty acid blend liquid A is discharged as a jet into the basic aqueous solution B in the mixing step.SELECTED DRAWING: Figure 9

Description

本発明は、脂肪酸中和物の製造方法に関する。 The present invention relates to a method for producing a neutralized fatty acid product.

液体石鹸の製造では、脂肪酸配合液と塩基性水溶液とを混合して脂肪酸をアルカリ剤で中和することにより脂肪酸中和物を生成させる。そして、そのような液体石鹸の製造方法として、例えば、特許文献1には、脂肪酸配合液と塩基性水溶液とを接触させ、それから1秒以内に、それらを細孔に流通させて混合することが開示されている。また、脂肪酸中和物を生成させる固形石鹸の製造方法として特許文献2には、脂肪酸配合液と塩基性水溶液とを2流体混合ノズルに供給し、その2流体混合ノズルから、それらの混合液を、透孔を有する隔壁で仕切られた複数の部屋のそれぞれに軸回転する撹拌羽根が設けられた装置内に噴射することが開示されている。 In the production of liquid soap, a fatty acid-neutralized product is produced by mixing a fatty acid-containing liquid and a basic aqueous solution and neutralizing the fatty acid with an alkaline agent. Then, as a method for producing such a liquid soap, for example, in Patent Document 1, a fatty acid mixture solution and a basic aqueous solution are brought into contact with each other, and within 1 second after that, they are passed through the pores and mixed. It is disclosed. Further, in Patent Document 2 as a method for producing a solid soap for producing a neutralized product of a fatty acid, a fatty acid mixture liquid and a basic aqueous solution are supplied to a two-fluid mixing nozzle, and the mixture liquid is mixed from the two-fluid mixing nozzle. It is disclosed that a plurality of chambers partitioned by a partition wall having a through hole are provided with an agitating blade that rotates about the axis to inject into a device.

特開2009−155529号公報JP, 2009-155529, A 特開昭59−20399号公報JP 59-20399 A

ところで、脂肪酸をアルカリ剤で中和して生成する脂肪酸中和物は、ゲル及びその凝集物を形成する。そして、この脂肪酸中和物のゲル及びその凝集物を溶解するのに時間を要する。そのため、脂肪酸中和物のゲル及びその凝集物の形成が、液体石鹸の製造効率を大きく下げる主要因となる。 By the way, a fatty acid neutralized product produced by neutralizing a fatty acid with an alkaline agent forms a gel and its aggregate. Then, it takes time to dissolve the gel of this fatty acid neutralized product and its aggregate. Therefore, the formation of gels of fatty acid neutralized products and their aggregates is a major factor that greatly reduces the production efficiency of liquid soap.

本発明の課題は、脂肪酸中和物のゲル及びその凝集物の形成が抑制される脂肪酸中和物の製造方法を提供することである。 An object of the present invention is to provide a gel of a neutralized fatty acid product and a method for producing a neutralized fatty acid product in which the formation of aggregates thereof is suppressed.

本発明は、脂肪酸配合液と塩基性水溶液とを混合する混合ステップを有する脂肪酸中和物の製造方法であって、前記混合ステップにおいて、前記脂肪酸配合液を前記塩基性水溶液に噴流状態で吐出させるものである。 The present invention is a method for producing a neutralized fatty acid product, which comprises a mixing step of mixing a fatty acid-mixed liquid and a basic aqueous solution, wherein in the mixing step, the fatty acid-mixed liquid is discharged into the basic aqueous solution in a jet state. It is a thing.

本発明によれば、脂肪酸配合液を塩基性水溶液に噴流状態で吐出させることにより、生成する脂肪酸中和物のゲル及びその凝集物の形成を抑制することができる。 According to the present invention, it is possible to suppress the formation of a gel of a fatty acid neutralized product to be formed and an aggregate thereof by ejecting the fatty acid-mixed liquid into the basic aqueous solution in a jet state.

実施形態1に係る脂肪酸中和物製造装置の構成を示す図である。It is a figure which shows the structure of the fatty-acid neutralized product manufacturing apparatus which concerns on Embodiment 1. 吐出ノズルの先端面の正面図である。It is a front view of the front end surface of the discharge nozzle. 吐出ノズルの先端部の縦断面図である。It is a longitudinal cross-sectional view of the tip portion of the discharge nozzle. 吐出ノズルの第1の変形例の先端面の正面図である。It is a front view of the front end surface of the 1st modification of a discharge nozzle. 吐出ノズルの第1の変形例の先端部の縦断面図である。It is a longitudinal cross-sectional view of the tip part of the 1st modification of a discharge nozzle. 吐出ノズルの第2の変形例の先端面の正面図である。It is a front view of the front end surface of the 2nd modification of a discharge nozzle. 吐出ノズルの第3の変形例の先端部の縦断面図である。It is a longitudinal cross-sectional view of the tip part of the 3rd modification of a discharge nozzle. 吐出ノズルの第4の変形例の先端面の正面図である。It is a front view of the front end surface of the 4th modification of a discharge nozzle. 吐出ノズルの第5の変形例の先端面の正面図である。It is a front view of the front end surface of the 5th modification of a discharge nozzle. 吐出ノズルの第6の変形例の先端面の正面図である。It is a front view of the front end surface of the 6th modification of a discharge nozzle. 脂肪酸配合液と塩基性水溶液との第1の混合態様を示す図である。It is a figure which shows the 1st mixing aspect of a fatty acid mixing liquid and a basic aqueous solution. 脂肪酸配合液と塩基性水溶液との第2の混合態様を示す図である。It is a figure which shows the 2nd mixing aspect of a fatty acid combination liquid and a basic aqueous solution. 脂肪酸配合液と塩基性水溶液との第3の混合態様を示す図である。It is a figure which shows the 3rd mixing aspect of a fatty acid mixing liquid and a basic aqueous solution. 脂肪酸配合液と塩基性水溶液との第4の混合態様を示す図である。It is a figure which shows the 4th mixing aspect of a fatty acid mixing liquid and a basic aqueous solution. 脂肪酸配合液と塩基性水溶液との第5の混合態様を示す図である。It is a figure which shows the 5th mixing aspect of a fatty acid mixing liquid and a basic aqueous solution. 脂肪酸配合液と塩基性水溶液との第6の混合態様を示す図である。It is a figure which shows the 6th mixing aspect of a fatty acid mixing liquid and a basic aqueous solution. 実施形態2に係る脂肪酸中和物製造装置の構成を示す図である。It is a figure which shows the structure of the fatty-acid neutralized substance manufacturing apparatus which concerns on Embodiment 2. 実施形態2に係る脂肪酸中和物製造装置の混合部の縦断面図である。It is a longitudinal cross-sectional view of the mixing part of the fatty-acid neutralized substance manufacturing apparatus which concerns on Embodiment 2. 実施形態3に係る脂肪酸中和物製造装置の混合部の縦断面図である。It is a longitudinal cross-sectional view of the mixing part of the fatty-acid neutralized product manufacturing apparatus which concerns on Embodiment 3. 実施形態4に係る脂肪酸中和物製造装置の構成を示す図である。It is a figure which shows the structure of the fatty-acid neutralized substance manufacturing apparatus which concerns on Embodiment 4. その他の実施形態の脂肪酸中和物製造装置の構成を示す図である。It is a figure which shows the structure of the fatty-acid neutralized substance manufacturing apparatus of other embodiment.

本発明は、脂肪酸配合液と塩基性水溶液とを混合する混合ステップを有する脂肪酸中和物の製造方法であって、前記混合ステップにおいて、前記脂肪酸配合液を前記塩基性水溶液に噴流状態で吐出させる脂肪酸中和物の製造方法である。 The present invention is a method for producing a neutralized fatty acid product, which comprises a mixing step of mixing a fatty acid-mixed liquid and a basic aqueous solution, wherein in the mixing step, the fatty acid-mixed liquid is discharged into the basic aqueous solution in a jet state. It is a method for producing a fatty acid neutralized product.

以下、各実施形態に共通して記載する。 Hereinafter, the description will be made commonly to each embodiment.

本発明の脂肪酸中和物の製造方法では、まず、脂肪酸配合液A及び塩基性原料水溶液Bを調製する。 In the method for producing a neutralized product of fatty acid of the present invention, first, the fatty acid mixture liquid A and the basic raw material aqueous solution B are prepared.

脂肪酸配合液Aは、脂肪酸を含有する。脂肪酸としては、例えば、カプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、ベヘニン酸、パーム核脂肪酸、ヤシ油脂肪酸、牛脂脂肪酸、純粋脂肪酸等が挙げられる。脂肪酸配合液Aは、これらのうちの1種又は2種以上の脂肪酸を含有することが好ましい。脂肪酸の炭素数は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは10以上、より好ましくは12以上であり、好ましくは24以下、より好ましくは22以下、更に好ましく18以下、更に好ましくは16以下である。 The fatty acid mixture liquid A contains a fatty acid. Examples of the fatty acid include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, palm kernel fatty acid, coconut oil fatty acid, tallow fatty acid, and pure fatty acid. The fatty acid mixture liquid A preferably contains one or more of these fatty acids. The carbon number of the fatty acid is preferably 10 or more, more preferably 12 or more, preferably 24 or less, more preferably 22 or less, still more preferably 18 from the viewpoint of suppressing formation of a gel of a fatty acid neutralized product and its aggregate. Or less, more preferably 16 or less.

脂肪酸配合液Aにおける脂肪酸の含有量は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは5質量%以上、より好ましくは20質量%以上、更に好ましくは40質量%以上であり、更に好ましくは60質量%以上であり、更に好ましくは80質量%以上であり、更に好ましくは90質量%以上であり、好ましくは99.5質量%以下、より好ましくは99質量%以下、更に好ましくは98.5質量%以下である。 The content of the fatty acid in the fatty acid mixture liquid A is preferably 5% by mass or more, more preferably 20% by mass or more, and further preferably 40% by mass or more, from the viewpoint of suppressing the formation of a gel of the fatty acid neutralized product and its aggregate. Is more preferably 60 mass% or more, further preferably 80 mass% or more, further preferably 90 mass% or more, preferably 99.5 mass% or less, more preferably 99 mass% or less, More preferably, it is 98.5 mass% or less.

脂肪酸配合液Aは、非イオン性界面活性剤を含有していてもよい。非イオン性界面活性剤としては、例えば、モノステアリン酸ポリエチレングリコール、モノオレイン酸ポリエチレングリコールなどのポリアルキレングリコール脂肪酸エステル;ポリオキシエチレンベヘニルエーテル、ポリオキシエチレンステアリルエーテルなどのポリオキシアルキレンアルキルエーテル等が挙げられる。脂肪酸配合液Aは、これらのうちの1種又は2種以上の非イオン性界面活性剤を含有していてもよく、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、ポリアルキレングリコール脂肪酸エステルを含有することが好ましく、モノステアリン酸ポリエチレングリコールを含有することがより好ましい。脂肪酸配合液Aにおける非イオン性界面活性剤の含有量は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは0.5質量%以上、より好ましくは1質量%以上、更に好ましくは1.5質量%以上であり、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは10質量%以下、より好ましくは5質量%以下、更に好ましくは3質量%、更に好ましくは2質量%以下である。 The fatty acid mixture solution A may contain a nonionic surfactant. Examples of the nonionic surfactant include polyalkylene glycol fatty acid esters such as polyethylene glycol monostearate and polyethylene glycol monooleate; polyoxyalkylene alkyl ethers such as polyoxyethylene behenyl ether and polyoxyethylene stearyl ether. Can be mentioned. The fatty acid mixture liquid A may contain one or more of these nonionic surfactants, and from the viewpoint of suppressing formation of a gel of fatty acid neutralized product and its aggregate, polyalkylene It is preferable to contain a glycol fatty acid ester, and it is more preferable to contain polyethylene glycol monostearate. The content of the nonionic surfactant in the fatty acid mixture solution A is preferably 0.5% by mass or more, more preferably 1% by mass or more, from the viewpoint of suppressing formation of a gel of fatty acid neutralized product and its aggregate. It is more preferably 1.5% by mass or more, and preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 3% by mass from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. , And more preferably 2% by mass or less.

脂肪酸配合液Aは、脂肪酸以外に、溶媒、清涼剤、保湿剤、酸化防止剤、電解質、非イオン性とせっけんを除く界面活性剤等を含有していてもよい。 The fatty acid-containing liquid A may contain a solvent, a cooling agent, a humectant, an antioxidant, an electrolyte, a nonionic surfactant and a surfactant other than soap, in addition to the fatty acid.

塩基性原料水溶液Bは、アルカリ剤を含有する。アルカリ剤としては、例えば、水酸化ナトリウム、水酸化カリウム、アミン化合物等が挙げられる。塩基性原料水溶液Bは、これらのうちの1種又は2種以上のアルカリ剤を含有することが好ましい。塩基性原料水溶液Bにおけるアルカリ剤の含有量は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは5質量%以上、より好ましくは7質量%以上、更に好ましくは8.5質量%以上であり、好ましくは50質量%以下、より好ましくは25質量%以下、更に好ましくは15質量%以下、更に好ましくは10質量%以下である。 The basic raw material aqueous solution B contains an alkaline agent. Examples of the alkaline agent include sodium hydroxide, potassium hydroxide, amine compounds and the like. The basic raw material aqueous solution B preferably contains one or more of these alkaline agents. The content of the alkaline agent in the basic raw material aqueous solution B is preferably 5% by mass or more, more preferably 7% by mass or more, and further preferably 8. From the viewpoint of suppressing the formation of gels of fatty acid neutralized products and aggregates thereof. It is 5% by mass or more, preferably 50% by mass or less, more preferably 25% by mass or less, further preferably 15% by mass or less, and further preferably 10% by mass or less.

塩基性原料水溶液Bは、水溶性溶剤を含有していてもよい。水溶性溶剤は、水と相溶性を有する溶剤であれば使用可能であるが、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくはポリオールから選択される1種又は2種以上、より好ましくはグリセリン及びポリグリセリンから選ばれる1種又は2種以上、更に好ましくはグリセリンである。塩基性原料水溶液Bにおける水溶性溶剤の含有量は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは5質量%以上、より好ましくは10質量%以上、更に好ましくは20質量%以上であり、更に好ましくは30質量%以上であり、好ましくは50質量%以下、より好ましくは42質量%以下、更に好ましくは35質量%以下である。 The basic raw material aqueous solution B may contain a water-soluble solvent. The water-soluble solvent can be used as long as it is a solvent having compatibility with water, but from the viewpoint of suppressing formation of a gel of a neutralized product of a fatty acid and its aggregate, one or two selected from polyols are preferable. As described above, one or more selected from glycerin and polyglycerin is more preferable, and glycerin is more preferable. The content of the water-soluble solvent in the basic raw material aqueous solution B is preferably 5% by mass or more, more preferably 10% by mass or more, and further preferably 20 from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. It is at least mass%, more preferably at least 30 mass%, preferably at most 50 mass%, more preferably at most 42 mass%, still more preferably at most 35 mass%.

塩基性原料水溶液Bは、アルカリ剤及び水以外に、電解質、界面活性剤、キレート剤等を含有していてもよい。 The basic raw material aqueous solution B may contain an electrolyte, a surfactant, a chelating agent, etc., in addition to the alkaline agent and water.

脂肪酸配合液Aの脂肪酸のモル数の塩基性原料水溶液Bの塩基のモル数に対するモル比(脂肪酸配合液Aの脂肪酸のモル数/塩基性原料水溶液Bの塩基のモル数)は、脂肪酸中和物を生成する観点から、好ましくは0.8以上、より好ましくは0.9以上であり、同様の観点から、好ましくは1.2以下、より好ましくは1.1以下である。 The molar ratio of the number of moles of fatty acid in the fatty acid mixture liquid A to the number of moles of base in the basic raw material aqueous solution B (the number of moles of fatty acid in the fatty acid mixture liquid A/the number of moles of base in the basic raw material aqueous solution B) is From the viewpoint of producing a product, it is preferably 0.8 or more, more preferably 0.9 or more, and from the same viewpoint, preferably 1.2 or less, more preferably 1.1 or less.

本願における「噴流状態」とは、塩基性水溶液B中に配置された孔から、脂肪酸配合液Aが塩基性水溶液Bに充たされた広い領域に噴き出し、孔径より小さい液滴が形成し、孔から拡散することが目視で確認できる状態をいう。 The “jet flow state” in the present application means that the fatty acid mixture solution A is ejected from a hole arranged in the basic aqueous solution B to a wide region filled with the basic aqueous solution B, and droplets smaller than the pore diameter are formed. The state in which it is possible to visually confirm that diffusion occurs.

また、この時の脂肪酸液滴径は、ゲル化及び凝集物を抑制する観点から、好ましくは300μm以下、より好ましくは100μm以下、更に好ましくは50μm以下であり、液滴の製造の容易性の観点から、好ましくは0.1μm以上、より好ましくは1μm以上、更に好ましくは5μm以上である。液滴径は、実施例記載の方法による測定することができる。 In addition, the fatty acid droplet size at this time is preferably 300 μm or less, more preferably 100 μm or less, further preferably 50 μm or less from the viewpoint of suppressing gelation and aggregates, and from the viewpoint of ease of manufacturing droplets. Therefore, it is preferably 0.1 μm or more, more preferably 1 μm or more, still more preferably 5 μm or more. The droplet size can be measured by the method described in Examples.

脂肪酸配合液Aの質量流量Xは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは0.5kg/min以上、より好ましくは0.7kg/min以上、更に好ましくは1kg/min以上であり、装置負荷を低減する観点から、好ましくは100kg/min以下、より好ましくは80kg/min以下、更に好ましくは60kg/min以下、更に好ましくは50kg/min以下である。 The mass flow rate X of the fatty acid-containing liquid A is preferably 0.5 kg/min or more, more preferably 0.7 kg/min or more, and further preferably 1 kg, from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. /Min or more, preferably 100 kg/min or less, more preferably 80 kg/min or less, further preferably 60 kg/min or less, and further preferably 50 kg/min or less from the viewpoint of reducing the load on the apparatus.

脂肪酸配合液Aの吐出方向の線速Vは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは1m/s以上、より好ましくは2m/s以上、更に好ましくは2.4m/s以上、更に好ましくは2.8m/s以上であり、装置負荷を低減する観点から、好ましくは50m/s以下、より好ましくは35m/s以下、更に好ましくは30m/s以下である。ここで、本出願における「吐出方向の線速」とは、脂肪酸配合液Aの吐出方向の吐出する向きにおける液体の速度である。また、この脂肪酸配合液Aの線速Vの絶対値は、脂肪酸配合液Aの質量流量Xを脂肪酸配合液Aの密度で除し、更にそれを吐出孔の面積で除し、それを1秒当たりに換算することにより算出される。 The linear velocity V A of the fatty acid mixture solution A in the discharge direction is preferably 1 m/s or more, more preferably 2 m/s or more, and further preferably 2 from the viewpoint of suppressing the formation of gels of fatty acid neutralized products and aggregates thereof. It is at least 0.4 m/s, more preferably at least 2.8 m/s, and from the viewpoint of reducing the load on the device, it is preferably at most 50 m/s, more preferably at most 35 m/s, still more preferably at most 30 m/s. .. Here, the “linear velocity in the ejection direction” in the present application is the velocity of the liquid in the ejection direction of the ejection direction of the fatty acid mixture liquid A. Further, the absolute value of the linear velocity V A of the fatty acid mixture liquid A is obtained by dividing the mass flow rate X of the fatty acid mixture liquid A by the density of the fatty acid mixture liquid A, and further dividing it by the area of the discharge hole. It is calculated by converting per second.

脂肪酸配合液Aの吐出部において、脂肪酸配合液Aの吐出方向の線速から、脂肪酸配合液Aの吐出方向における塩基性水溶液Bの線速を減じた線速差で定義される脂肪酸相対線速ΔVは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは1m/s以上、より好ましくは2m/s以上、更に好ましくは2.4m/s以上、更に好ましくは2.8m/s以上であり、設備負荷を低減する観点から、好ましくは50m/s以下であり、より好ましくは35m/s以下、更に好ましくは30m/s以下である。 In the discharge part of the fatty acid mixture A, the relative linear velocity of fatty acid defined by the linear velocity difference obtained by subtracting the linear velocity of the basic aqueous solution B in the discharge direction of the fatty acid mixture A from the linear velocity in the discharge direction of the fatty acid mixture A. ΔV is preferably 1 m/s or more, more preferably 2 m/s or more, still more preferably 2.4 m/s or more, and further preferably 2. From the viewpoint of suppressing the formation of gel of fatty acid neutralized product and its aggregate. It is 8 m/s or more, and from the viewpoint of reducing equipment load, it is preferably 50 m/s or less, more preferably 35 m/s or less, and further preferably 30 m/s or less.

塩基性水溶液Bが非流動状態にある場合、図7Aに示すように、塩基性水溶液Bの線速Vは0m/sであるので、この脂肪酸相対線速ΔVは、脂肪酸配合液Aの吐出方向の線速Vである。塩基性水溶液Bが、撹拌等により流動状態にある場合、脂肪酸配合液Aの吐出方向と塩基性水溶液Bの流動方向との関係により、脂肪酸相対線速ΔVは以下のようになる。図7Bに示すように、流速Vで吐出する脂肪酸配合液Aに対し、その吐出方向に直交する方向に塩基性水溶液Bが流速Vで流動する場合、塩基性水溶液Bの線速Vのうちの脂肪酸配合液Aの吐出方向における成分VBx=0m/sであるので、この脂肪酸相対線速ΔVも、脂肪酸配合液Aの吐出方向の線速Vである。 When the basic aqueous solution B is in a non-flowing state, as shown in FIG. 7A, the linear velocity V B of the basic aqueous solution B is 0 m/s. Direction linear velocity V A. When the basic aqueous solution B is in a fluid state due to stirring or the like, the fatty acid relative linear velocity ΔV is as follows depending on the relationship between the discharge direction of the fatty acid-containing solution A and the flowing direction of the basic aqueous solution B. As shown in FIG. 7B, when the basic aqueous solution B flows at a flow rate V B in a direction orthogonal to the discharge direction with respect to the fatty acid mixture solution A discharged at a flow rate V A , the linear velocity V B of the basic aqueous solution B. Of these components, the component V Bx =0 m/s in the discharge direction of the fatty acid mixture liquid A, the relative fatty acid linear velocity ΔV is also the linear velocity V A of the fatty acid mixture liquid A in the discharge direction.

図7Cに示すように、流速Vで吐出する脂肪酸配合液Aに対し、その吐出方向に同一の向きに塩基性水溶液Bが流速Vで流動する場合、この脂肪酸相対線速ΔVは、脂肪酸配合液Aの吐出方向の線速Vから塩基性水溶液Bの線速Vを減じたものである。又は、図7Dに示すように、流速Vで吐出する脂肪酸配合液Aに対し、その吐出方向に反対の向きに塩基性水溶液Bが流速Vで流動する場合、この脂肪酸相対線速ΔVは、脂肪酸配合液Aの吐出方向の線速Vからに塩基性水溶液Bの線速Vを加算し減じたものである。 As shown in FIG. 7C, when the basic aqueous solution B flows at the flow rate V B in the same direction as the discharge direction of the fatty acid mixture solution A discharged at the flow rate V A , the fatty acid relative linear velocity ΔV is It is obtained by subtracting the linear velocity V B of the basic aqueous solution B from the linear velocity V A of the mixed solution A in the discharge direction. Alternatively, as shown in FIG. 7D, when the basic aqueous solution B flows at the flow rate V B in the direction opposite to the discharge direction with respect to the fatty acid mixture solution A discharged at the flow rate V A , the fatty acid relative linear velocity ΔV is is minus the sum of the linear velocity V B of the basic aqueous solution B from the linear velocity V a of the discharge direction of a fatty acid blend solution a.

図7Eに示すように、流速Vで吐出する脂肪酸配合液Aに対し、その吐出方向に傾斜した方向の前方から塩基性水溶液Bが流速Vで流動する場合、又は、図7Fに示すように、流速Vで吐出する脂肪酸配合液Aに対し、その吐出方向に傾斜した方向の後方から塩基性水溶液Bが流速Vで流動する場合、この脂肪酸相対線速ΔVは、脂肪酸配合液Aの吐出方向の線速Vから、塩基性水溶液Bの線速Vのうち脂肪酸配合液Aの吐出方向における成分VBxを減じたものである。なお、これらの脂肪酸配合液Aの吐出方向及び吐出の向きは、吐出ノズル14の設置態様によって自在に設定することができる。 As shown in FIG. 7E, when the basic aqueous solution B flows at a flow rate V B from the front in the direction inclined with respect to the fatty acid mixture solution A discharged at a flow rate V A , or as shown in FIG. 7F. When the basic aqueous solution B flows at the flow velocity V B from the rear of the fatty acid mixture liquid A discharged at the flow velocity V A , the fatty acid relative linear velocity ΔV is the discharge direction of the linear velocity V a of, those obtained by subtracting the component V Bx in the direction of ejection of the fatty acid blended solution a of the linear velocity V B of the basic aqueous solution B. The discharge direction and the discharge direction of these fatty acid-containing liquids A can be freely set depending on the installation mode of the discharge nozzle 14.

以下、実施形態について詳細に説明する。 Hereinafter, embodiments will be described in detail.

(実施形態1)
図1は、実施形態1に係る脂肪酸中和物製造装置10を示す。
(Embodiment 1)
FIG. 1 shows a fatty acid neutralized product manufacturing apparatus 10 according to the first embodiment.

実施形態1に係る脂肪酸中和物製造装置10は、脂肪酸配合液Aを貯留するための脂肪酸槽11及び塩基性水溶液Bを貯留するための塩基槽12と、脂肪酸槽11の底部から延びて塩基槽12の上部に結合して差し入れられた脂肪酸供給配管13とを備える。なお、脂肪酸供給配管13は、塩基槽12の側部又は底部に結合して差し入れられていてもよい。脂肪酸槽11及び塩基槽12のそれぞれには、図示しない撹拌機構及び温調機構が設けられている。脂肪酸供給配管13には送液ポンプPが介設されているとともに、塩基槽12内に導入された脂肪酸供給配管13の先端には吐出ノズル14が取り付けられている。 The fatty acid neutralized product manufacturing apparatus 10 according to the first embodiment includes a fatty acid tank 11 for storing the fatty acid mixture solution A, a base tank 12 for storing the basic aqueous solution B, and a base extending from the bottom of the fatty acid tank 11. And a fatty acid supply pipe 13 inserted and connected to the upper part of the tank 12. The fatty acid supply pipe 13 may be inserted and connected to the side portion or the bottom portion of the base tank 12. Each of the fatty acid tank 11 and the base tank 12 is provided with a stirring mechanism and a temperature control mechanism (not shown). A liquid feed pump P is provided in the fatty acid supply pipe 13, and a discharge nozzle 14 is attached to the tip of the fatty acid supply pipe 13 introduced into the base tank 12.

図2A及びBは、吐出ノズル14の先端部を示す。吐出ノズル14の先端部は、円筒状の管端で構成されており、孔径φが管内径に等しい丸孔状の吐出孔15を有する。吐出孔15の孔径φは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは0.5mm以上、より好ましくは0.7mm以上、更に好ましくは1mm以上であり、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは20mm以下、より好ましくは15mm以下、更に好ましくは10mm以下、更に好ましくは5mm以下、更に好ましくは2mm以下である。なお、吐出ノズル14の先端部は、図3A及びBに示すように、吐出孔15の孔径φが管内径よりも小さく縮小されていてもよい。この場合、吐出孔15は、先端面の中央ではなく、図4に示すように、偏心して設けられていてもよい。また、吐出ノズル14の先端部は、図5に示すように、半球状等に形成されていてもよい。さらに、吐出ノズル14の先端部における吐出孔15の孔形状は、図6Aに示すようなスリット状であってもよく、図6Bに示すような円弧孔状であってもよく、図6Cに示すような細長三角孔状であってもよい。このように吐出孔15の孔形状が非円形の場合、その孔径φは、吐出孔15の面積が同一の等価円の直径が相当する。 2A and 2B show the tip of the discharge nozzle 14. The tip of the discharge nozzle 14 is formed of a cylindrical tube end, and has a round hole-shaped discharge hole 15 having a hole diameter φ equal to the inner diameter of the tube. The diameter φ of the discharge hole 15 is preferably 0.5 mm or more, more preferably 0.7 mm or more, still more preferably 1 mm or more from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. From the viewpoint of suppressing the formation of a Japanese gel and its aggregate, it is preferably 20 mm or less, more preferably 15 mm or less, still more preferably 10 mm or less, still more preferably 5 mm or less, still more preferably 2 mm or less. As shown in FIGS. 3A and 3B, the tip diameter of the discharge nozzle 14 may be such that the hole diameter φ of the discharge hole 15 is smaller than the inner diameter of the pipe. In this case, the discharge hole 15 may be eccentrically provided, as shown in FIG. 4, instead of the center of the tip surface. Further, the tip of the discharge nozzle 14 may be formed in a hemispherical shape or the like, as shown in FIG. Further, the hole shape of the discharge hole 15 at the tip of the discharge nozzle 14 may be a slit shape as shown in FIG. 6A, an arc hole shape as shown in FIG. 6B, or the hole shape shown in FIG. 6C. It may be in the shape of an elongated triangular hole. When the discharge hole 15 has a non-circular shape in this way, the hole diameter φ corresponds to the diameter of an equivalent circle having the same area of the discharge hole 15.

次に、実施形態1に係る脂肪酸中和物の製造方法について説明する。 Next, a method for producing a fatty acid neutralized product according to the first embodiment will be described.

実施形態1に係る脂肪酸中和物の製造方法は、脂肪酸配合液Aと塩基性水溶液Bとを混合する混合ステップを有する。前記混合ステップにおいて、前記脂肪酸配合液Aを前記塩基性水溶液Bに噴流状態で吐出させる。また、前記混合ステップを、塩基槽12内の塩基性水溶液B中に前記脂肪酸配合液Aを流動させて行う。 The method for producing a fatty acid neutralized product according to the first embodiment includes a mixing step of mixing the fatty acid mixture liquid A and the basic aqueous solution B. In the mixing step, the fatty acid mixture solution A is jetted into the basic aqueous solution B in a jet state. Further, the mixing step is performed by causing the fatty acid mixture solution A to flow into the basic aqueous solution B in the base tank 12.

実施形態1に係る脂肪酸中和物の製造方法では、まず、脂肪酸配合液A及び塩基性原料水溶液Bを前述のとおり調製する。 In the method for producing a fatty acid neutralized product according to the first embodiment, first, the fatty acid mixture liquid A and the basic raw material aqueous solution B are prepared as described above.

次いで、脂肪酸配合液A及び塩基性原料水溶液Bを、それぞれ脂肪酸槽11及び塩基槽12に仕込む。このとき、塩基槽12では、吐出ノズル14が塩基性原料水溶液B中に配置されるようにする。脂肪酸配合液A及び塩基性原料水溶液Bの液温は、例えば40℃以上90℃以下とする。脂肪酸槽11における脂肪酸配合液Aの液温は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは40℃以上、より好ましくは50℃以上、更に好ましくは60℃以上であり、装置負荷を低減する観点から、好ましくは90℃以下、より好ましくは80℃以下である。塩基槽12における塩基性原料水溶液Bの液温は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは40℃以上、より好ましくは45℃以上であり、装置負荷を低減する観点から、好ましくは90℃以下、より好ましくは60℃以下、更に好ましくは50℃以下である。これらの液温は、同一であっても、異なっていても、どちらでもよい。なお、塩基性原料水溶液は、脂肪酸配合液が混合されると組成が変化するので、本出願では、初期の塩基性原料水溶液及びそれに脂肪酸配合液を混合した液のいずれも含めて「塩基性水溶液」という。 Next, the fatty acid mixture solution A and the basic raw material aqueous solution B are charged into the fatty acid tank 11 and the base tank 12, respectively. At this time, in the base tank 12, the discharge nozzle 14 is arranged in the basic raw material aqueous solution B. The liquid temperature of the fatty acid mixture liquid A and the basic raw material aqueous solution B is, for example, 40° C. or higher and 90° C. or lower. The liquid temperature of the fatty acid-containing liquid A in the fatty acid tank 11 is preferably 40° C. or higher, more preferably 50° C. or higher, further preferably 60° C. or higher from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. From the viewpoint of reducing the load on the apparatus, the temperature is preferably 90° C. or lower, more preferably 80° C. or lower. The liquid temperature of the basic raw material aqueous solution B in the base tank 12 is preferably 40° C. or higher, and more preferably 45° C. or higher, from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof, thus reducing the load on the apparatus. From this viewpoint, the temperature is preferably 90°C or lower, more preferably 60°C or lower, and further preferably 50°C or lower. These liquid temperatures may be the same, different, or either. In addition, since the composition of the basic raw material aqueous solution changes when the fatty acid mixed solution is mixed, in the present application, both the initial basic raw material aqueous solution and the liquid obtained by mixing the fatty acid mixed solution are referred to as “basic aqueous solution”. ".

そして、送液ポンプPを稼働させて脂肪酸槽11の脂肪酸配合液Aを脂肪酸供給配管13を介して塩基槽12に送り、脂肪酸配合液Aを吐出ノズル14の先端部の吐出孔15から塩基性水溶液Bに噴流状態で吐出させて、脂肪酸配合液Aと塩基性水溶液Bとを混合する(混合ステップ)。このとき、脂肪酸がアルカリ剤で中和されて脂肪酸中和物を生成することとなり、バッチ操作により脂肪酸中和物が製造される。 Then, the liquid feed pump P is operated to feed the fatty acid mixed solution A in the fatty acid tank 11 to the base tank 12 through the fatty acid supply pipe 13, and the fatty acid mixed solution A is basic from the discharge hole 15 at the tip of the discharge nozzle 14. The aqueous solution B is discharged in a jet state to mix the fatty acid mixture solution A and the basic aqueous solution B (mixing step). At this time, the fatty acid is neutralized with an alkaline agent to form a fatty acid neutralized product, and the fatty acid neutralized product is produced by batch operation.

このような実施形態1に係る脂肪酸中和物の製造方法によれば、脂肪酸配合液Aと塩基性水溶液Bとを混合する混合ステップを含み、その混合ステップにおいて、脂肪酸配合液Aを塩基性水溶液Bに噴流状態で吐出させることにより、生成する脂肪酸中和物のゲル及びその凝集物の形成を抑制することができる。この脂肪酸中和物のゲル及びその凝集物の形成抑制効果は、脂肪酸配合液Aが噴流状態で塩基性水溶液Bに吐出されると、脂肪酸配合液Aが塩基性水溶液B中に分散する液滴を形成することが関与しているものと推測される。ここで、噴流状態にするには、塩基性水溶液B中で、脂肪酸配合液Aを吐出する必要がある。 The method for producing a neutralized fatty acid product according to Embodiment 1 includes a mixing step of mixing the fatty acid mixture liquid A and the basic aqueous solution B, and in the mixing step, the fatty acid mixture liquid A is mixed with the basic aqueous solution. When B is discharged in a jet state, it is possible to suppress the formation of the gel of the fatty acid neutralized product to be formed and the aggregate thereof. The effect of suppressing the formation of the gel of the fatty acid neutralized product and the aggregate thereof is that the fatty acid mixed solution A is dispersed in the basic aqueous solution B when the fatty acid mixed solution A is jetted to the basic aqueous solution B. It is speculated that the formation of Here, in order to form a jet flow, it is necessary to discharge the fatty acid mixture solution A in the basic aqueous solution B.

実施形態1や後述する実施形態2等では、バッチ操作により、塩基性水溶液B中に脂肪酸配合液Aを吐出することから、反応初期では、塩基性水溶液B中の塩基のモル数が、吐出される脂肪酸配合液A中の脂肪酸のモル数より過剰にあるため中和反応が進行し易いが、反応後期では、塩基性水溶液B中に脂肪酸中和物が生成し、塩基性水溶液B中の塩基のモル数が減少するため、反応が進行し難くなると考えられる。しかしながら、脂肪酸配合液Aが液滴を形成することで、反応が進み易くなり、ゲルの生成を抑制できたと推定される。尚、ゲルは、主として、未中和の脂肪酸が凝集したものと推定される。 In Embodiment 1 and Embodiment 2 which will be described later, since the fatty acid mixture liquid A is discharged into the basic aqueous solution B by a batch operation, the number of moles of the base in the basic aqueous solution B is discharged in the initial stage of the reaction. The neutralization reaction is likely to proceed because it is in excess of the number of moles of the fatty acid in the fatty acid mixture solution A. However, in the latter stage of the reaction, a neutralized fatty acid product is formed in the basic aqueous solution B, and the base in the basic aqueous solution B is generated. It is considered that the reaction becomes difficult to proceed because the number of moles of is decreased. However, it is presumed that the fatty acid-containing solution A formed droplets to facilitate the reaction and suppress the formation of gel. The gel is presumed to be mainly agglomerated of unneutralized fatty acids.

脂肪酸配合液Aを吐出するとき、塩基性水溶液Bは、塩基槽12の撹拌機構を稼働させない非流動状態であっても、塩基槽12の撹拌機構を稼働させた流動状態であっても、どちらでもよい。 When the fatty acid mixture solution A is discharged, the basic aqueous solution B may be in a non-fluid state in which the stirring mechanism of the base tank 12 is not operated or in a fluid state in which the stirring mechanism of the base tank 12 is operated. But it's okay.

脂肪酸配合液Aの質量流量Xは、前述のとおりである。 The mass flow rate X of the fatty acid mixture liquid A is as described above.

脂肪酸配合液Aの吐出部、つまり、吐出ノズル14の先端部における吐出孔15の開口部において、脂肪酸配合液Aの吐出方向の線速Vは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは1m/s以上、より好ましくは2m/s以上、更に好ましくは2.4m/s以上、更に好ましくは2.8m/s以上、更に好ましくは10m/s以上、更に好ましくは20m/s以上、更に好ましくは25m/s以上であり、装置負荷を低減する観点から、好ましくは50m/s以下、より好ましくは35m/s以下、更に好ましくは30m/s以下である。 At the discharge part of the fatty acid mixture A, that is, at the opening of the discharge hole 15 at the tip of the discharge nozzle 14, the linear velocity V A in the discharge direction of the fatty acid mixture A is the gel of fatty acid neutralized product and its aggregates. From the viewpoint of suppressing formation, it is preferably 1 m/s or more, more preferably 2 m/s or more, still more preferably 2.4 m/s or more, further preferably 2.8 m/s or more, further preferably 10 m/s or more, It is preferably 20 m/s or more, more preferably 25 m/s or more, and from the viewpoint of reducing the device load, it is preferably 50 m/s or less, more preferably 35 m/s or less, and further preferably 30 m/s or less.

脂肪酸配合液Aの吐出部において、脂肪酸配合液Aの吐出方向の線速から、脂肪酸配合液Aの吐出方向における塩基性水溶液Bの線速を減じた線速差で定義される脂肪酸相対線速ΔVは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは1m/s以上、より好ましくは2m/s以上、更に好ましくは15m/s以上、更に好ましくは30m/s以上であり、設備負荷を低減する観点から、好ましくは50m/s以下であり、より好ましくは35m/s以下である。 In the discharge part of the fatty acid mixture A, the relative linear velocity of fatty acid defined by the linear velocity difference obtained by subtracting the linear velocity of the basic aqueous solution B in the discharge direction of the fatty acid mixture A from the linear velocity in the discharge direction of the fatty acid mixture A. ΔV is preferably 1 m/s or more, more preferably 2 m/s or more, further preferably 15 m/s or more, further preferably 30 m/s or more, from the viewpoint of suppressing formation of gel of fatty acid neutralized product and its aggregate. From the viewpoint of reducing equipment load, it is preferably 50 m/s or less, and more preferably 35 m/s or less.

(実施形態2)
図8は、実施形態2に係る脂肪酸中和物製造装置10を示す。なお、実施形態1と同一名称の部分は、実施形態1及び2と同一符号で示す。
(Embodiment 2)
FIG. 8 shows a fatty acid neutralized product manufacturing apparatus 10 according to the second embodiment. The parts having the same names as those in the first embodiment are designated by the same reference numerals as those in the first and second embodiments.

実施形態2に係る脂肪酸中和物製造装置10は、脂肪酸配合液Aを貯留するための脂肪酸槽11及び塩基性水溶液Bを貯留するための塩基槽12と、塩基槽12の底部から延びて同じ塩基槽12の側部に結合して差し入れられた循環配管16と、循環配管16に介設された混合部17と、脂肪酸槽11から延びて混合部17に結合した脂肪酸供給配管13とを備える。なお、循環配管16は、塩基槽12の上部又は底部に結合して差し入れられていてもよい。脂肪酸槽11及び塩基槽12のそれぞれには、図示しない撹拌機構及び温調機構が設けられている。循環配管16における塩基槽12の底部から混合部17まで間の部分には第1の送液ポンプPが介設されている。脂肪酸供給配管13には第2の送液ポンプPが介設されている。 The fatty acid neutralized product manufacturing apparatus 10 according to the second embodiment is the same as the fatty acid tank 11 for storing the fatty acid mixture solution A and the base tank 12 for storing the basic aqueous solution B, which extends from the bottom of the base tank 12 and is the same. The base pipe 12 is provided with a circulation pipe 16 inserted and connected to the side portion, a mixing unit 17 interposed in the circulation pipe 16, and a fatty acid supply pipe 13 extending from the fatty acid bath 11 and connected to the mixing unit 17. .. The circulation pipe 16 may be inserted and connected to the top or bottom of the base tank 12. Each of the fatty acid tank 11 and the base tank 12 is provided with a stirring mechanism and a temperature control mechanism (not shown). A first liquid feed pump P 1 is provided in a portion of the circulation pipe 16 between the bottom portion of the base tank 12 and the mixing portion 17. The fatty acid supply pipe 13 is provided with a second liquid feed pump P 2 .

図9は、混合部17を示す。この混合部17は、循環配管16に脂肪酸供給配管13が結合するとともに差し入れられて同心状に設けられた二重管で構成されている。循環配管16の内径Φは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは10mm以上、より好ましくは15mm以上、更に好ましくは20mm以上であり、好ましくは200mm以下、より好ましくは150mm以下、更に好ましくは110mm以下である。循環配管16の流路形状が非円形の場合、その内径Φは、流路面積が同一の等価円の直径が相当する。脂肪酸供給配管13の先端部は、実施形態1の吐出ノズル14の先端部と同様、円筒状の管端で構成されており、孔径φが脂肪酸供給配管13の内径に等しい丸孔状の吐出孔15を有する。 FIG. 9 shows the mixing section 17. The mixing section 17 is composed of a double pipe in which the fatty acid supply pipe 13 is connected to the circulation pipe 16 and is inserted and concentrically provided. The inner diameter Φ of the circulation pipe 16 is preferably 10 mm or more, more preferably 15 mm or more, further preferably 20 mm or more, and more preferably 200 mm or less, from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. It is preferably 150 mm or less, more preferably 110 mm or less. When the flow passage shape of the circulation pipe 16 is non-circular, the inner diameter Φ corresponds to the diameter of an equivalent circle having the same flow passage area. Similar to the tip of the discharge nozzle 14 of the first embodiment, the tip of the fatty acid supply pipe 13 is formed of a cylindrical pipe end, and the hole diameter φ is a round hole-shaped discharge hole equal to the inner diameter of the fatty acid supply pipe 13. Have 15.

吐出孔15の孔径φは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは0.5mm以上、より好ましくは0.7mm以上、更に好ましくは1mm以上であり、好ましくは20mm以下、より好ましくは15mm以下、更に好ましくは10mm以下である。なお、脂肪酸供給配管13は、循環配管16に対して偏心して設けられていてもよい。また、脂肪酸供給配管13の先端部は、図3A及びB、図4、並びに図5に示す実施形態1の吐出ノズル14の先端部の変形例と同様の構成を有していてもよい。さらに、脂肪酸供給配管13の先端部における吐出孔15の孔形状も、図6A〜Cに示す実施形態1の吐出ノズル14の先端部における吐出孔15の孔形状の変形例と同様の構成を有していてもよい。 The hole diameter φ of the discharge hole 15 is preferably 0.5 mm or more, more preferably 0.7 mm or more, still more preferably 1 mm or more, from the viewpoint of suppressing formation of a gel of fatty acid neutralized product and its aggregate. It is 20 mm or less, more preferably 15 mm or less, and further preferably 10 mm or less. The fatty acid supply pipe 13 may be provided eccentrically with respect to the circulation pipe 16. Further, the tip portion of the fatty acid supply pipe 13 may have the same configuration as the modification of the tip portion of the discharge nozzle 14 of the first embodiment shown in FIGS. 3A and 3B, FIG. 4 and FIG. Further, the hole shape of the discharge hole 15 at the tip portion of the fatty acid supply pipe 13 also has the same configuration as the modified example of the hole shape of the discharge hole 15 at the tip portion of the discharge nozzle 14 of Embodiment 1 shown in FIGS. You may have.

次に、実施形態2に係る脂肪酸中和物の製造方法について説明する。 Next, a method for producing a neutralized fatty acid product according to the second embodiment will be described.

実施形態2に係る脂肪酸中和物の製造方法は、脂肪酸配合液と塩基性水溶液とを混合する混合ステップを有する。そして、前記混合ステップにおいて、前記脂肪酸配合液を前記塩基性水溶液に噴流状態で吐出させる。また、前記混合ステップを配管内で前記脂肪酸配合液及び前記塩基性水溶液のそれぞれを流動させて行う。 The method for producing a fatty acid-neutralized product according to the second embodiment includes a mixing step of mixing the fatty acid-containing solution and the basic aqueous solution. Then, in the mixing step, the fatty acid-containing solution is jetted into the basic aqueous solution in a jet state. Further, the mixing step is performed by flowing the fatty acid mixture solution and the basic aqueous solution in a pipe.

実施形態2に係る脂肪酸中和物の製造方法では、まず、脂肪酸配合液A及び塩基性原料水溶液Bを調製し、それぞれ脂肪酸槽11及び塩基槽12に仕込む。 In the method for producing a fatty acid neutralized product according to the second embodiment, first, the fatty acid mixture liquid A and the basic raw material aqueous solution B are prepared and charged into the fatty acid tank 11 and the base tank 12, respectively.

そして、第1の送液ポンプPを稼働させて塩基槽12に貯留された塩基性水溶液Bを、循環配管16に、塩基槽12の底部から流出して側部に戻るように循環させる。また、第2の送液ポンプPを稼働させて脂肪酸槽11の脂肪酸配合液Aを脂肪酸供給配管13を介して循環配管16内に送液し、混合部17において、脂肪酸配合液Aを脂肪酸供給配管13の先端部の吐出孔15から循環配管16内を流動する塩基性水溶液Bに噴流状態で吐出させて、脂肪酸配合液Aと塩基性水溶液Bとを混合する(混合ステップ)。したがって、循環配管16内で脂肪酸配合液A及び塩基性水溶液Bのそれぞれを流動させて混合ステップを行う。また、このとき、脂肪酸がアルカリ剤で中和されて脂肪酸中和物を生成することとなり、バッチ操作により脂肪酸中和物が製造される。 Then, the first liquid feed pump P 1 is operated to circulate the basic aqueous solution B stored in the base tank 12 through the circulation pipe 16 so as to flow out from the bottom portion of the base tank 12 and return to the side portion. Further, the second liquid feed pump P 2 is operated to feed the fatty acid mixture liquid A in the fatty acid tank 11 into the circulation pipe 16 via the fatty acid supply pipe 13, and the fatty acid mixture liquid A is converted into the fatty acid in the mixing section 17. The fatty acid mixture solution A and the basic aqueous solution B are mixed by jetting the basic aqueous solution B flowing in the circulation pipe 16 from the discharge hole 15 at the tip of the supply pipe 13 in a jet state (mixing step). Therefore, each of the fatty acid mixture solution A and the basic aqueous solution B is caused to flow in the circulation pipe 16 to perform the mixing step. Further, at this time, the fatty acid is neutralized with an alkaline agent to form a fatty acid neutralized product, and the fatty acid neutralized product is produced by batch operation.

脂肪酸配合液Aの吐出部において、脂肪酸配合液Aの吐出孔15の孔径φに対する塩基性水溶液Bが流動する循環配管16の内径Φの比(Φ/φ)は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは4以上、より好ましくは5.5以上、更に好ましくは7以上であり、好ましくは30以下、より好ましくは20以下、更に好ましくは12以下である。 In the discharge part of the fatty acid mixture liquid A, the ratio (Φ/φ) of the inner diameter Φ of the circulation pipe 16 through which the basic aqueous solution B flows to the hole diameter φ of the discharge hole 15 of the fatty acid mixture liquid A is the gel of the fatty acid neutralized product and From the viewpoint of suppressing the formation of the aggregate, it is preferably 4 or more, more preferably 5.5 or more, still more preferably 7 or more, preferably 30 or less, more preferably 20 or less, still more preferably 12 or less.

脂肪酸配合液Aの質量流量Xは、前述の通りである。 The mass flow rate X of the fatty acid mixture liquid A is as described above.

塩基性水溶液Bの質量流量Yは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは5kg/min以上、より好ましくは7kg/min以上、更に好ましくは8kg/min以上であり、装置負荷を低減する観点から、好ましくは1500kg/min以下、より好ましくは1000kg/min以下、更に好ましくは800kg/min以下である。 The mass flow rate Y of the basic aqueous solution B is preferably 5 kg/min or more, more preferably 7 kg/min or more, and further preferably 8 kg/min or more from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. From the viewpoint of reducing the load on the apparatus, it is preferably 1500 kg/min or less, more preferably 1000 kg/min or less, still more preferably 800 kg/min or less.

脂肪酸配合液Aの吐出部において、脂肪酸配合液Aの質量流量Xに対する塩基性水溶液Bの質量流量Yの比(Y/X)は、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは5以上、より好ましくは7以上、更に好ましくは8以上であり、好ましくは50以下、より好ましくは30以下、更に好ましくは20以下である。 The ratio (Y/X) of the mass flow rate Y of the basic aqueous solution B to the mass flow rate X of the fatty acid blended solution A at the discharge part of the fatty acid blended solution A is (Y/X) from the viewpoint of suppressing formation of a gel of fatty acid neutralized product and its aggregate. Therefore, it is preferably 5 or more, more preferably 7 or more, still more preferably 8 or more, preferably 50 or less, more preferably 30 or less, still more preferably 20 or less.

脂肪酸配合液Aの質量流量Xに対する塩基性水溶液Bの質量流量Yの比(Y/X)は、経時において、変更してもよい。製造途中で、(Y/X)を1回以上増加させることが、ゲル化物の生成の抑制及び製造時間短縮の観点から好ましい。具体的には、全脂肪酸配合液量の好ましくは60質量%以上、より好ましくは70質量%以上、更に好ましくは80質量%以上吐出させた後に、脂肪酸配合液Aの質量流量を減少させる、若しくは、塩基性水溶液Bの質量流量を増加させる、又は、その両方を行うことで、Y/Xを増加させることが、ゲル化物の生成の抑制及び製造時間短縮の観点から好ましい。Y/Xの増加量は、ゲル化物の生成の抑制及び製造時間短縮の観点から、好ましくは1以上、より好ましくは5以上であり、装置負荷を低減する観点から、好ましくは20以下、より好ましくは10以下である。 The ratio (Y/X) of the mass flow rate Y of the basic aqueous solution B to the mass flow rate X of the fatty acid mixture solution A may be changed over time. It is preferable to increase (Y/X) once or more during the production from the viewpoint of suppressing the formation of a gelled product and shortening the production time. Specifically, the mass flow rate of the fatty acid blended liquid A is reduced after discharging preferably 60 mass% or more, more preferably 70 mass% or more, still more preferably 80 mass% or more of the total amount of the fatty acid blended liquid, or It is preferable to increase Y/X by increasing the mass flow rate of the basic aqueous solution B, or by performing both of them, from the viewpoint of suppressing the formation of a gelled product and shortening the manufacturing time. The amount of increase in Y/X is preferably 1 or more, more preferably 5 or more, from the viewpoint of suppressing the formation of a gelled product and shortening the manufacturing time, and preferably 20 or less, more preferably from the viewpoint of reducing the device load. Is 10 or less.

噴流場に供給される、単位時間当たりのモル比(塩基/脂肪酸)が大きくなるように、吐出する脂肪酸配合液Aの質量流量Xに対する、循環する塩基性水溶液Bの質量流量Yの比(Y/X)を増加させることで、反応が進行し易くなり、ゲル化物の生成も抑制される。 The ratio (Y) of the mass flow rate Y of the circulating basic aqueous solution B to the mass flow rate X of the fatty acid mixture solution A to be discharged so that the molar ratio (base/fatty acid) supplied to the jet field becomes large. By increasing /X), the reaction is facilitated and the formation of a gelled product is suppressed.

脂肪酸配合液Aの吐出部、つまり、脂肪酸供給配管13の先端部における吐出孔15の開口部において、脂肪酸配合液Aの吐出方向の線速Vは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは1m/s以上、より好ましくは2m/s以上、更に好ましくは2.4m/s以上、更に好ましくは2.8m/s以上であり、装置負荷を低減する観点から、好ましくは50m/s以下、より好ましくは35m/s以下、更に好ましくは30m/s以下、更に好ましくは15m/s以下、更に好ましくは13m/s以下である。この脂肪酸配合液Aの線速Vの絶対値は、脂肪酸配合液Aの質量流量Xを脂肪酸配合液Aの密度で除し、更にそれを吐出孔15の面積で除し、それを1秒当たりに換算することにより算出される。 At the discharge part of the fatty acid mixture A, that is, at the opening of the discharge hole 15 at the tip of the fatty acid supply pipe 13, the linear velocity V A in the discharge direction of the fatty acid mixture A is the gel of fatty acid neutralized product and its aggregate. From the viewpoint of suppressing the formation of 1), it is preferably 1 m/s or more, more preferably 2 m/s or more, still more preferably 2.4 m/s or more, still more preferably 2.8 m/s or more, and a viewpoint of reducing the device load. Therefore, it is preferably 50 m/s or less, more preferably 35 m/s or less, further preferably 30 m/s or less, further preferably 15 m/s or less, further preferably 13 m/s or less. The absolute value of the linear velocity VA of the fatty acid mixture liquid A is obtained by dividing the mass flow rate X of the fatty acid mixture liquid A by the density of the fatty acid mixture liquid A and further dividing it by the area of the discharge hole 15 for 1 second. It is calculated by converting per hit.

脂肪酸配合液Aの吐出部において、脂肪酸配合液Aの吐出方向における塩基性水溶液Bの線速Vは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは0.1m/s以上、より好ましくは0.2m/s以上、更に好ましくは0.3m/s以上、更に好ましくは0.4m/s以上であり、装置負荷を低減する観点から、好ましくは4m/s以下、より好ましくは2m/s以下、更に好ましくは1.5m/s以下である。この塩基性水溶液Bの線速Vの絶対値は、塩基性水溶液Bの質量流量Yを塩基性原料水溶液Bの密度で除し、更にそれを循環配管16の管内の面積から吐出孔15の面積を引いた流路面積で除し、それを1秒当たりに換算することにより算出される。 In the discharge part of the fatty acid mixture A, the linear velocity V B of the basic aqueous solution B in the discharge direction of the fatty acid mixture A is preferably 0.1 m from the viewpoint of suppressing formation of a gel of fatty acid neutralized product and its aggregate. /S or more, more preferably 0.2 m/s or more, further preferably 0.3 m/s or more, further preferably 0.4 m/s or more, and preferably 4 m/s or less from the viewpoint of reducing the load on the device. , More preferably 2 m/s or less, still more preferably 1.5 m/s or less. The absolute value of the linear velocity V B of the basic aqueous solution B is obtained by dividing the mass flow rate Y of the basic aqueous solution B by the density of the basic raw material aqueous solution B, and further dividing it by the area inside the pipe of the circulation pipe 16 of the discharge hole 15. It is calculated by dividing the area by the flow path area minus the area and converting it per second.

実施形態2に係る脂肪酸中和物の製造方法では、実施形態1における図7Cに示すのと同様、線速Vで流動する塩基性水溶液Bに対し、その流動方向に同一の向きに脂肪酸配合液Aを線速Vで吐出することとなる。したがって、脂肪酸相対線速ΔVは、脂肪酸配合液Aの吐出方向の線速Vから塩基性水溶液Bの線速Vを減じたものと等しい。この場合、脂肪酸相対線速ΔVは、脂肪酸中和物のゲル及びその凝集物の形成抑制の観点から、好ましくは1m/s以上、より好ましくは2m/s以上、更に好ましくは2.2m/s以上、更に好ましくは2.4m/s以上、更に好ましくは2.8m/s以上であり、設備負荷を低減する観点から、好ましくは50m/s以下、より好ましくは35m/s以下、更に好ましくは30m/s以下、更に好ましくは15m/s以下、更に好ましくは13m/s以下である。 In the method for producing a fatty acid neutralized product according to the second embodiment, similar to that shown in FIG. 7C in the first embodiment, the basic aqueous solution B flowing at the linear velocity V B is mixed with the fatty acid in the same direction in the flowing direction. The liquid A is discharged at the linear velocity V A. Thus, fatty acids relative linear velocity ΔV is equal to minus the linear velocity V B of the basic aqueous solution B from the linear velocity V A of the discharge direction of a fatty acid blend solution A. In this case, the fatty acid relative linear velocity ΔV is preferably 1 m/s or more, more preferably 2 m/s or more, and further preferably 2.2 m/s, from the viewpoint of suppressing formation of gels of fatty acid neutralized products and aggregates thereof. Or more, more preferably 2.4 m/s or more, further preferably 2.8 m/s or more, and preferably 50 m/s or less, more preferably 35 m/s or less, and further preferably from the viewpoint of reducing equipment load. It is 30 m/s or less, more preferably 15 m/s or less, and further preferably 13 m/s or less.

その他の構成及び作用効果は実施形態1と同一である。 The other configurations and operational effects are the same as those of the first embodiment.

(実施形態3)
図10は、実施形態3に係る脂肪酸中和物製造装置10における混合部17を示す。なお、実施形態1及び2と同一名称の部分は、実施形態1と同一符号で示す。
(Embodiment 3)
FIG. 10 shows the mixing unit 17 in the fatty acid neutralized product manufacturing apparatus 10 according to the third embodiment. The parts having the same names as those in the first and second embodiments are indicated by the same reference numerals as those in the first embodiment.

この混合部17は、循環配管16に脂肪酸供給配管13が垂直に結合して構成されている。そして、循環配管16の内壁における脂肪酸供給配管13の開口が、孔径φが脂肪酸供給配管13の内径に等しい丸孔状の吐出孔15を構成している。なお、脂肪酸供給配管13の循環配管16への結合端部は、図3A及びBに示す実施形態1の吐出ノズル14の先端部の変形例と同様に吐出孔15の孔径φが脂肪酸供給配管13の内径よりも小さく縮小されていてもよい。また脂肪酸供給配管13の循環配管16への結合端部における吐出孔15の孔形状は、図6A〜Cに示す実施形態1の吐出ノズル14の先端部における吐出孔15の孔形状の変形例と同様の構成を有していてもよい。その他の構成は、実施形態2に係る脂肪酸中和物製造装置10と同一である。 The mixing unit 17 is configured by vertically connecting the fatty acid supply pipe 13 to the circulation pipe 16. The opening of the fatty acid supply pipe 13 on the inner wall of the circulation pipe 16 constitutes a round hole-shaped discharge hole 15 having a hole diameter φ equal to the inner diameter of the fatty acid supply pipe 13. The fatty acid supply pipe 13 is connected to the circulation pipe 16 at the end of the fatty acid supply pipe 13 in which the diameter φ of the discharge hole 15 is the same as in the modification of the tip of the discharge nozzle 14 of the first embodiment shown in FIGS. 3A and 3B. It may be reduced to be smaller than the inner diameter of. Further, the hole shape of the discharge hole 15 at the end of the fatty acid supply pipe 13 connected to the circulation pipe 16 is a modification of the hole shape of the discharge hole 15 at the tip of the discharge nozzle 14 of Embodiment 1 shown in FIGS. You may have the same structure. Other configurations are the same as those of the fatty acid neutralized product manufacturing apparatus 10 according to the second embodiment.

実施形態3に係る脂肪酸中和物の製造方法では、実施形態2の場合と同様、バッチ操作により脂肪酸中和物が製造される。このとき、実施形態1における図7Bに示すのと同様、線速Vで流動する塩基性水溶液Bに対し、その流動方向に直交する方向から脂肪酸配合液Aを吐出することとなるので、脂肪酸相対線速ΔVは、脂肪酸配合液Aの吐出方向の線速Vと等しい。 In the method for producing a fatty acid neutralized product according to the third embodiment, as in the case of the second embodiment, the fatty acid neutralized product is produced by batch operation. At this time, similarly to the case shown in FIG. 7B in the first embodiment, the fatty acid-containing liquid A is discharged from the direction orthogonal to the flowing direction with respect to the basic aqueous solution B flowing at the linear velocity V B. The relative linear velocity ΔV is equal to the linear velocity V A of the fatty acid mixture solution A in the ejection direction.

その他の構成及び作用効果は実施形態1及び2と同一である。好ましい数値範囲は、実施形態2と同一である。 Other configurations and operational effects are the same as those of the first and second embodiments. The preferable numerical range is the same as that of the second embodiment.

(実施形態4)
図11は、実施形態4に係る脂肪酸中和物製造装置10を示す。なお、実施形態1及び2と同一名称の部分は、実施形態1及び2と同一符号で示す。
(Embodiment 4)
FIG. 11 shows a fatty acid neutralized product manufacturing apparatus 10 according to the fourth embodiment. The parts having the same names as those in the first and second embodiments are denoted by the same reference numerals as those in the first and second embodiments.

実施形態4に係る脂肪酸中和物製造装置10では、循環配管16における混合部17から塩基槽12の側部までの間の部分に剪断付与部18が設けられている。剪断付与部18は、循環配管16よりも流路面積が狭小な部分を有し、その部分に、混合部17で脂肪酸配合液Aが混合された塩基性水溶液Bを流通させて剪断を付与する。これにより、脂肪酸配合液Aと塩基性水溶液Bとの混合で生成する脂肪酸中和物のゲル及びその凝集物の形成抑制をより効果的に図ることができる。剪断付与部18は、多種の脂肪酸及びアルカリ剤の組み合わせに対応して、流路面積を自在に設定できるという観点から、バルブのような流路面積が可変である装置要素で構成されていることが好ましい。但し、剪断付与部18は、流路面積が固定された静止型混合器等で構成されていてもよい。 In the fatty acid neutralized product manufacturing apparatus 10 according to the fourth embodiment, a shearing unit 18 is provided in a portion of the circulation pipe 16 between the mixing unit 17 and the side portion of the base tank 12. The shearing part 18 has a part having a smaller flow passage area than the circulation pipe 16, and the basic aqueous solution B mixed with the fatty acid mixture A in the mixing part 17 is circulated to the part to give shearing. .. This makes it possible to more effectively suppress the formation of a gel of a fatty acid neutralized product produced by mixing the fatty acid mixture liquid A and the basic aqueous solution B and the aggregate thereof. The shearing unit 18 is composed of a device element such as a valve whose flow passage area is variable, from the viewpoint that the flow passage area can be freely set corresponding to combinations of various fatty acids and alkaline agents. Is preferred. However, the shearing unit 18 may be composed of a static mixer or the like having a fixed flow passage area.

その他の構成及び作用効果は実施形態1及び2と同一である。なお、混合部17は、実施形態3の構成のものであってもよい。好ましい数値範囲は、実施形態2と同一である。 Other configurations and operational effects are the same as those of the first and second embodiments. The mixing unit 17 may have the configuration of the third embodiment. The preferable numerical range is the same as that of the second embodiment.

(その他の実施形態)
上記実施形態1〜4では、バッチ操作での脂肪酸中和物の製造方法を示したが、特にこれに限定されるものではなく、図12に示すような脂肪酸中和物製造装置10を用いた連続操作での脂肪酸中和物の製造方法であってもよい。具体的には、図12に示す脂肪酸中和物製造装置10では、脂肪酸槽11から延びる脂肪酸供給配管13a及び塩基槽12から延びる塩基供給配管13bがそれぞれ混合部17に結合し、混合部17から延びる回収配管19が回収槽20の上部に結合して差し入れられている。そして、脂肪酸槽11及び塩基槽12にそれぞれ脂肪酸配合液A及び塩基性原料水溶液Bを仕込み、脂肪酸供給配管13a及び塩基供給配管13bのそれぞれに介設された送液ポンプPを稼働させると、混合部17において、脂肪酸配合液Aが塩基性水溶液Bに噴流状態で吐出され、それらが混合されて脂肪酸中和物を生成し、その脂肪酸中和物を含む反応液Cが回収配管19を介して回収槽20に連続的に回収される。好ましい数値範囲は、実施形態2と同一である。
(Other embodiments)
In the above-mentioned Embodiments 1 to 4, the method for producing a fatty acid neutralized product by a batch operation is shown, but the present invention is not particularly limited to this, and a fatty acid neutralized product producing apparatus 10 as shown in FIG. 12 is used. It may be a method for producing a neutralized fatty acid product by continuous operation. Specifically, in the fatty acid neutralized product manufacturing apparatus 10 shown in FIG. 12, the fatty acid supply pipe 13 a extending from the fatty acid tank 11 and the base supply pipe 13 b extending from the base tank 12 are respectively coupled to the mixing unit 17, and from the mixing unit 17. An extending recovery pipe 19 is inserted and connected to the upper part of the recovery tank 20. Then, the fatty acid mixture solution A and the basic raw material aqueous solution B are charged in the fatty acid tank 11 and the base tank 12, respectively, and the liquid feed pump P provided in each of the fatty acid supply pipe 13a and the base supply pipe 13b is operated to mix them. In the part 17, the fatty acid mixture solution A is jetted into the basic aqueous solution B in a jet state, and they are mixed to produce a fatty acid neutralized product, and the reaction solution C containing the fatty acid neutralized product is passed through the recovery pipe 19. It is continuously collected in the collecting tank 20. The preferable numerical range is the same as that of the second embodiment.

(脂肪酸配合液A及び塩基性原料水溶液Bの調製)
表1に示す配合で脂肪酸配合液Aを調製した。また、表2−1に示す配合で塩基性原料水溶液Bを調製した。
(Preparation of fatty acid mixture solution A and basic raw material aqueous solution B)
A fatty acid mixture liquid A was prepared according to the formulation shown in Table 1. In addition, a basic raw material aqueous solution B was prepared according to the formulation shown in Table 2-1.

用いた原料は以下のとおりである。
ラウリン酸 ルナックL-98:花王社製
ミリスチン酸 ルナックMY-98:花王社製
パルミチン酸 ルナックP-95:花王社製
モノステアリン酸ポリエチレングリコール エマノーン3199VB:花王社製
48%水酸化カリウム液 液体苛性カリ(48%):旭硝子社製
グリセリン 化粧品用濃グリセリン:花王社製
The raw materials used are as follows.
Lauric acid Lunak L-98: Kao company myristic acid Lunak MY-98: Kao company palmitate Lunac P-95: Kao company monostearate polyethylene glycol Emanone 3199VB: Kao company 48% potassium hydroxide liquid liquid caustic ( 48%): Asahi Glass Co., Ltd. Glycerin Cosmetic concentrated glycerin: Kao

Figure 2020100809
Figure 2020100809

Figure 2020100809
Figure 2020100809

(脂肪酸中和物の製造及び評価方法)
上記脂肪酸配合液A及び塩基性原料水溶液Bを用いて次の実施例1〜9及び比較例の脂肪酸中和物の製造を行った。それぞれの結果及び製造条件を、表3及び4に示す。
(Production and evaluation method of fatty acid neutralized product)
Using the fatty acid mixture liquid A and the basic raw material aqueous solution B, fatty acid neutralized products of the following Examples 1 to 9 and Comparative Example were produced. The respective results and manufacturing conditions are shown in Tables 3 and 4.

また、評価は、以下の方法で行った。 The evaluation was performed by the following method.

噴流状態の有無の確認は目視にて行った。 The presence/absence of the jet state was visually confirmed.

ゲルの有無は下記の基準で、目視にて行った。
無:脂肪酸中和物製造時に、脂肪酸中和物のゲル及びその凝集物の形成は認められなかった。
少し有:少量の脂肪酸中和物のゲル及びその凝集物の形成が認められた。
有:脂肪酸中和物のゲル及びその凝集物の形成が明確に認められた。
The presence or absence of gel was visually observed according to the following criteria.
None: At the time of producing the neutralized product of fatty acid, formation of gel of the neutralized product of fatty acid and its aggregate was not observed.
Some Yes: A small amount of gel of fatty acid neutralized product and its aggregate were formed.
Existence: Formation of gel of fatty acid neutralized product and its aggregate was clearly observed.

実施例1については、脂肪酸液滴径を測定した。このとき、噴流時の脂肪酸の液滴径を測定するため、塩基性原料水溶液Bを、表2−2に示す水溶液Cに変更した。これは、塩基性原料水溶液Bを用いた場合、噴流により形成された脂肪酸液滴が中和の進行とともに消失するため、安定した液滴径の測定が困難なためである。水溶液Cは、グリセリンと精製水の質量比が、塩基性原料水溶液Bにおけるグリセリンと精製水の質量比と一致する組成である。また、形成した液滴径の安定化のため、ポリビニルアルコール(ゴーセノールEG-05C:三菱ケミカル社製)を1%添加した。 For Example 1, the fatty acid droplet size was measured. At this time, the basic raw material aqueous solution B was changed to the aqueous solution C shown in Table 2-2 in order to measure the droplet diameter of the fatty acid at the time of jetting. This is because when the basic raw material aqueous solution B is used, the fatty acid droplets formed by the jet flow disappear as the neutralization progresses, making it difficult to stably measure the droplet diameter. The aqueous solution C has a composition in which the mass ratio of glycerin to purified water is the same as the mass ratio of glycerin to purified water in the basic raw material aqueous solution B. Further, 1% of polyvinyl alcohol (GOHSENOL EG-05C: manufactured by Mitsubishi Chemical Corporation) was added to stabilize the diameter of the formed droplets.

Figure 2020100809
Figure 2020100809

脂肪酸配合液Aを水溶液Cに噴流状態で吐出し、形成された脂肪酸液滴を含む乳化液の一部を採取し、直ちにその液滴径を測定した。結果及び製造条件を表3に示す。
測定条件:
(1)測定装置:レーザー回折型粒径測定機「LA−960」(株式会社堀場製作所製)
(2)測定条件:測定用セルに水を加え、吸光度が適正範囲になる濃度で体積中位粒径(D50)を測定した。なお相対屈折率1.20、温度25℃、循環ポンプON、循環速度5とした。
The fatty acid-mixed liquid A was jetted into the aqueous solution C in a jet state, a part of the emulsion containing the formed fatty acid droplets was collected, and the droplet diameter was immediately measured. The results and manufacturing conditions are shown in Table 3.
Measurement condition:
(1) Measuring device: Laser diffraction type particle size measuring device "LA-960" (manufactured by Horiba Ltd.)
(2) Measurement conditions: Water was added to the measurement cell, and the volume median particle diameter (D 50 ) was measured at a concentration such that the absorbance was in the appropriate range. The relative refractive index was 1.20, the temperature was 25° C., the circulation pump was ON, and the circulation speed was 5.

<実施例1>
上記実施形態1と同一構成の脂肪酸中和物製造装置10であって、吐出ノズル14の吐出孔15が鉛直下向きに開口したものを用い、その脂肪酸槽11及び塩基槽12にそれぞれ上記脂肪酸配合液A及び塩基性原料水溶液Bを仕込み、塩基槽12内で撹拌している塩基性水溶液B内に吐出ノズル14の吐出孔15から脂肪酸配合液Aを噴流状態で吐出させて脂肪酸中和物を製造した。したがって、脂肪酸配合液Aと塩基性水溶液Bとの混合態様は、図7Bに示すのと同様、撹拌により流動する塩基性水溶液Bに対し、その流動方向に直交する方向から脂肪酸配合液Aを吐出するものである。なお、脂肪酸配合液Aの脂肪酸のモル数の塩基性原料水溶液Bの塩基のモル数に対するモル比は1.01(脂肪酸/塩基)であった。
<Example 1>
A fatty acid neutralized product manufacturing apparatus 10 having the same configuration as that of Embodiment 1 is used, in which the discharge holes 15 of the discharge nozzles 14 are opened vertically downward, and the fatty acid mixture liquid is contained in the fatty acid tank 11 and the base tank 12, respectively. A and a basic raw material aqueous solution B are charged, and the fatty acid-containing solution A is jetted into the basic aqueous solution B stirred in the base tank 12 from the discharge hole 15 of the discharge nozzle 14 to produce a fatty acid neutralized product. did. Therefore, in the mixing mode of the fatty acid mixture liquid A and the basic aqueous solution B, the fatty acid mixture liquid A is discharged from the direction orthogonal to the flowing direction with respect to the basic aqueous solution B that flows by stirring, as in the case shown in FIG. 7B. To do. The molar ratio of the number of moles of fatty acid in the fatty acid mixture solution A to the number of moles of base in the basic raw material aqueous solution B was 1.01 (fatty acid/base).

実施例1において、脂肪酸液滴径の測定を行った。上記塩基性水溶液Bを水溶液Cに変更した以外は、同じ条件で噴流した。脂肪酸液滴平均径は、14.1μmであった。 In Example 1, the fatty acid droplet diameter was measured. Jetting was performed under the same conditions except that the basic aqueous solution B was changed to the aqueous solution C. The fatty acid droplet average diameter was 14.1 μm.

<実施例2、3>
上記実施形態2と同一構成の脂肪酸中和物製造装置10を用い、その脂肪酸槽11及び塩基槽12にそれぞれ上記脂肪酸配合液A及び塩基性原料水溶液Bを仕込み、循環配管16を循環している塩基性水溶液B内に、二重管の混合部17で、吐出孔15から脂肪酸配合液Aを噴流状態で吐出させて脂肪酸中和物を製造した。したがって、脂肪酸配合液Aと塩基性水溶液Bとの混合態様は、図7Cに示すのと同様、流動する塩基性水溶液Bに対し、その流動方向に同一の向きに脂肪酸配合液Aを吐出するものである。なお、脂肪酸配合液Aの脂肪酸のモル数の塩基性原料水溶液Bの塩基のモル数に対するモル比は1.01(脂肪酸/塩基)であった。
<Examples 2 and 3>
The fatty acid neutralized product manufacturing apparatus 10 having the same configuration as that of the second embodiment is used, and the fatty acid tank 11 and the base tank 12 are charged with the fatty acid mixture solution A and the basic raw material aqueous solution B, respectively, and circulated through the circulation pipe 16. A fatty acid-neutralized product was produced by discharging the fatty acid-containing liquid A in a jet state into the basic aqueous solution B from the discharge hole 15 in the double tube mixing section 17. Therefore, in the mixing mode of the fatty acid mixture liquid A and the basic aqueous solution B, the fatty acid mixture liquid A is discharged in the same direction as the flowing basic aqueous solution B as in the case shown in FIG. 7C. Is. The molar ratio of the number of moles of fatty acid in the fatty acid mixture solution A to the number of moles of base in the basic raw material aqueous solution B was 1.01 (fatty acid/base).

<実施例4〜8>
上記実施形態4と同一構成の脂肪酸中和物製造装置10であって、上記実施形態2と同一構成の二重管の混合部17と、バルブの剪断付与部18とを備えたものを用い、その脂肪酸槽11及び塩基槽12にそれぞれ上記脂肪酸配合液A及び塩基性原料水溶液Bを仕込み、バルブの剪断付与部18の開度と送液ポンプP2の出力により塩基性水溶液Bの質量流量Yを調整し、循環配管16を循環している塩基性水溶液B内に、二重管の混合部17で、吐出孔15から脂肪酸配合液Aを噴流状態で吐出させて脂肪酸中和物を製造した。なお、実施例4〜6では、脂肪酸配合液Aの脂肪酸のモル数の塩基性原料水溶液Bの塩基のモル数に対するモル比は1.01(脂肪酸/塩基)であった。実施例7及び8では、脂肪酸配合液Aの脂肪酸のモル数の塩基性原料水溶液Bの塩基のモル数に対するモル比は1.02(脂肪酸/塩基)であった。
<Examples 4 to 8>
A fatty acid neutralized product manufacturing apparatus 10 having the same configuration as that of the above-described Embodiment 4, which is provided with a double pipe mixing unit 17 and a valve shearing unit 18 having the same configuration as that of Embodiment 2 above, The fatty acid mixture solution A and the basic raw material aqueous solution B are charged in the fatty acid tank 11 and the base tank 12, respectively, and the mass flow rate Y of the basic aqueous solution B is determined by the opening degree of the shearing unit 18 of the valve and the output of the liquid feed pump P2. A fatty acid-neutralized product was prepared by discharging the fatty acid-containing solution A in a jet state from the discharge hole 15 into the basic aqueous solution B which was circulated and circulated in the circulation pipe 16 in the mixing section 17 of the double pipe. In Examples 4 to 6, the molar ratio of the number of moles of the fatty acid in the fatty acid mixture solution A to the number of moles of the base in the basic raw material aqueous solution B was 1.01 (fatty acid/base). In Examples 7 and 8, the molar ratio of the number of moles of fatty acid in the fatty acid mixture solution A to the number of moles of base in the basic raw material aqueous solution B was 1.02 (fatty acid/base).

実施例3と実施例6とを比較すると、流量比のY/Xを除いてほぼ同じ条件で実施しているが、実施例3では得られた脂肪酸中和物にゲル凝集物が少し見られたのに対し、Y/Xが小さいにも関わらず、実施例6ではゲル凝集物が見られなかった。これは、実施例6の図11の装置が剪断付与部を有しているためと考えられる。 When Example 3 and Example 6 are compared, it is carried out under substantially the same conditions except for the flow rate ratio Y/X, but in Example 3, a little gel aggregate is observed in the obtained fatty acid neutralized product. On the other hand, in Example 6, no gel aggregate was found even though Y/X was small. It is considered that this is because the device of FIG. 11 of Example 6 has a shear applying part.

実施例4〜6を比較すると、実施例4では得られた脂肪酸中和物にゲル凝集物が少し見られたが、これは流量比のY/Xが7.0と小さいためと考えられる。 When Examples 4 to 6 were compared with each other, a small amount of gel aggregate was found in the obtained fatty acid neutralized product, which is considered to be because the flow ratio Y/X was as small as 7.0.

<実施例9>
投入開始から所定投入量の80質量%を吐出するまでの間、脂肪酸配合液Aの質量流量を61.5kg/minとし、製造途中の所定投入量の80質量%を吐出した時点で、質量流量を40kg/minに変化させて脂肪酸中和物を製造し、塩基性水溶液Bの質量流量は常に800kg/minで一定とした以外は、実施例4と同様に脂肪酸中和物を製造した。なお、脂肪酸配合液Aの脂肪酸のモル数の塩基性原料水溶液Bの塩基のモル数に対するモル比は1.02(脂肪酸/塩基)であった。
<Example 9>
The mass flow rate of the fatty acid blended liquid A was 61.5 kg/min from the start of charging until the discharge of 80 mass% of the predetermined charging amount, and the mass flow rate at the time of discharging 80 mass% of the predetermined charging amount during manufacturing. Was changed to 40 kg/min to produce a neutralized fatty acid, and the neutralized fatty acid was produced in the same manner as in Example 4 except that the mass flow rate of the basic aqueous solution B was constantly kept at 800 kg/min. The molar ratio of the number of moles of fatty acid in the fatty acid mixture solution A to the number of moles of base in the basic raw material aqueous solution B was 1.02 (fatty acid/base).

噴流場に供給される、脂肪酸中和物の所定投入量の80質量%を吐出した際の、吐出する脂肪酸配合液Aの質量流量Xに対する塩基性水溶液Bの質量流量Yの比(Y/X)は、13であり、質量流量変更後の比は20であり、したがって、Y/Xの増加量は7であった。 The ratio (Y/X) of the mass flow rate Y of the basic aqueous solution B to the mass flow rate X of the fatty acid mixture solution A to be discharged when 80% by mass of the predetermined amount of the fatty acid neutralized substance supplied to the jet field is discharged. ) Was 13 and the ratio after changing the mass flow rate was 20, and therefore the increase in Y/X was 7.

実施例7〜9を比較すると、得られた脂肪酸中和物に、いずれもゲル凝集物が見られなかったが、製造途中に流量比Y/Xを変更した実施例9は、製造時間が短くできた。即ち、反応開始直後は、ゲル凝集物は出来にくいため、脂肪酸流量を大きくしてY/Xを小さくし、反応後期に脂肪酸流量を小さくしてY/Xを大きくすることで、ゲル凝集物を抑制する方が、製造時間が短縮されることがわかる。尚、実施例7、8,9の製造時間は、それぞれ、15.0分、9.0分、8.1分であり、実施例7、実施例8と比較して、それぞれ46%、10%の時間短縮であった。 Comparing Examples 7 to 9, no gel aggregates were found in the obtained fatty acid neutralized products, but in Example 9 in which the flow rate ratio Y/X was changed during the production, the production time was short. did it. That is, since it is difficult to form gel aggregates immediately after the start of the reaction, by increasing the fatty acid flow rate to reduce Y/X and decreasing the fatty acid flow rate to increase Y/X in the latter stage of the reaction, gel aggregates are formed. It can be seen that the suppression suppresses the manufacturing time. The manufacturing times of Examples 7, 8 and 9 were 15.0 minutes, 9.0 minutes and 8.1 minutes, respectively, which were 46% and 10%, respectively, as compared with Examples 7 and 8. It was a% time reduction.

<比較例>
液槽に上記塩基性原料水溶液Bを仕込み、その液槽内で撹拌している塩基性原料水溶液B中に、管内径80mmの配管端から上記脂肪酸配合液Aを上面から注いで脂肪酸中和物を製造した。このとき、脂肪酸中和物のゲル及びその凝集物の形成が明確に認められた。なお、このときの脂肪酸配合液Aの質量流量Xは40kg/min及び線速は0.13m/sにそれぞれ相当する。
<Comparative example>
A fatty acid neutralized product is prepared by charging the above-mentioned basic raw material aqueous solution B into a liquid tank and pouring the above-mentioned fatty acid-containing solution A into the basic raw material aqueous solution B which is being stirred in the liquid tank from the pipe end having a pipe inner diameter of 80 mm. Was manufactured. At this time, the formation of gel of fatty acid neutralized product and its aggregate was clearly observed. The mass flow rate X of the fatty acid mixture solution A at this time corresponds to 40 kg/min and the linear velocity corresponds to 0.13 m/s, respectively.

Figure 2020100809
Figure 2020100809

Figure 2020100809
Figure 2020100809

本発明は、脂肪酸中和物の製造方法の技術分野について有用である。 INDUSTRIAL APPLICABILITY The present invention is useful in the technical field of a method for producing a fatty acid neutralized product.

10 脂肪酸中和物製造装置
11 脂肪酸槽
12 塩基槽
13,13a 脂肪酸供給配管
13b 塩基供給配管
14 吐出ノズル
15 吐出孔
16 循環配管
17 混合部
18 剪断付与部
19 回収配管
20 回収槽
A 脂肪酸配合液
B 塩基性原料水溶液、塩基性水溶液
C 反応液
P,P,P 送液ポンプ
10 Fatty Acid Neutralized Product Manufacturing Apparatus 11 Fatty Acid Tank 12 Base Tank 13, 13a Fatty Acid Supply Pipe 13b Base Supply Pipe 14 Discharge Nozzle 15 Discharge Hole 16 Circulation Pipe 17 Mixing Section 18 Shearing Section 19 Recovery Pipe 20 Recovery Tank A Fatty Acid Mixture B Basic raw material aqueous solution, basic aqueous solution C Reaction liquid P, P 1 , P 2 liquid feed pump

Claims (10)

脂肪酸配合液と塩基性水溶液とを混合する混合ステップを有する脂肪酸中和物の製造方法であって、
前記混合ステップにおいて、前記脂肪酸配合液を前記塩基性水溶液に噴流状態で吐出させる脂肪酸中和物の製造方法。
A method for producing a fatty acid neutralized product, which comprises a mixing step of mixing a fatty acid-containing liquid and a basic aqueous solution,
In the mixing step, a method for producing a neutralized fatty acid product, wherein the fatty acid-containing liquid is jetted into the basic aqueous solution in a jet flow state.
前記脂肪酸配合液の吐出部において、前記脂肪酸配合液の吐出方向の線速から、前記脂肪酸配合液の吐出方向における前記塩基性水溶液の線速を減じた脂肪酸相対線速が1m/s以上である、請求項1に記載された脂肪酸中和物の製造方法。 In the discharge part of the fatty acid mixture, the relative linear velocity of fatty acid obtained by subtracting the linear velocity of the basic aqueous solution in the discharge direction of the fatty acid mixture from the linear velocity in the discharge direction of the fatty acid mixture is 1 m/s or more. A method for producing a fatty acid neutralized product according to claim 1. 前記脂肪酸配合液の吐出部において、前記脂肪酸配合液の吐出方向の線速が1m/s以上である、請求項1又は2に記載された脂肪酸中和物の製造方法。 The method for producing a neutralized fatty acid product according to claim 1 or 2, wherein a linear velocity in a discharging direction of the fatty acid mixed liquid is 1 m/s or more in a discharge portion of the fatty acid mixed liquid. 前記噴流状態では、前記塩基性水溶液中に、脂肪酸の液滴が形成される、請求項1乃至3のいずれかに記載の脂肪酸中和物の製造方法。 The method for producing a neutralized fatty acid product according to claim 1, wherein in the jet state, fatty acid droplets are formed in the basic aqueous solution. 前記混合ステップを、前記塩基性水溶液中に前記脂肪酸配合液を流動させて行う、 請求項1乃至4のいずれかに記載された脂肪酸中和物の製造方法。 The method for producing a fatty acid neutralized product according to any one of claims 1 to 4, wherein the mixing step is performed by causing the fatty acid mixture solution to flow in the basic aqueous solution. 前記混合ステップを配管内で前記脂肪酸配合液及び前記塩基性水溶液のそれぞれを流動させて行う、請求項1乃至5のいずれかに記載された脂肪酸中和物の製造方法。 The method for producing a neutralized fatty acid product according to any one of claims 1 to 5, wherein the mixing step is performed by flowing each of the fatty acid mixture liquid and the basic aqueous solution in a pipe. 前記脂肪酸配合液の吐出部において、前記脂肪酸配合液の質量流量に対する前記塩基性水溶液の質量流量の比が5以上である、請求項6に記載された脂肪酸中和物の製造方法。 The method for producing a fatty acid neutralized product according to claim 6, wherein the ratio of the mass flow rate of the basic aqueous solution to the mass flow rate of the fatty acid mixture solution is 5 or more in the discharge section of the fatty acid mixture solution. 前記脂肪酸配合液の吐出部において、前記脂肪酸配合液の吐出孔の孔径に対する前記塩基性水溶液が流動する配管の内径の比が4以上である、請求項6又は7に記載された脂肪酸中和物の製造方法。 8. The fatty acid neutralized product according to claim 6 or 7, wherein a ratio of an inner diameter of a pipe through which the basic aqueous solution flows is 4 or more with respect to a diameter of a discharge hole of the fatty acid mixture, in the discharge part of the fatty acid mixture. Manufacturing method. 前記脂肪酸配合液の質量流量に対する前記塩基性水溶液の質量流量の比を増加させる、請求項6乃至8のいずれかに記載の脂肪酸中和物の製造方法。 The method for producing a fatty acid neutralized product according to claim 6, wherein the ratio of the mass flow rate of the basic aqueous solution to the mass flow rate of the fatty acid mixture liquid is increased. 前記脂肪酸配合液を60質量%以上吐出させた後に、前記脂肪酸配合液の質量流量に対する前記塩基性水溶液の質量流量の比を増加させる、請求項9に記載の脂肪酸中和物の製造方法。 The method for producing a fatty acid neutralized product according to claim 9, wherein the ratio of the mass flow rate of the basic aqueous solution to the mass flow rate of the fatty acid mixture solution is increased after discharging the fatty acid mixture solution by 60 mass% or more.
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