KR20230006102A - Method for manufacturing dispersant - Google Patents
Method for manufacturing dispersant Download PDFInfo
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- KR20230006102A KR20230006102A KR1020210086846A KR20210086846A KR20230006102A KR 20230006102 A KR20230006102 A KR 20230006102A KR 1020210086846 A KR1020210086846 A KR 1020210086846A KR 20210086846 A KR20210086846 A KR 20210086846A KR 20230006102 A KR20230006102 A KR 20230006102A
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- phosphoric acid
- reactor
- temperature
- dispersant
- tde
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- 239000002270 dispersing agent Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 31
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 9
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 7
- 229940087291 tridecyl alcohol Drugs 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- NKSOSPOXQKNIKJ-CLFAGFIQSA-N Polyoxyethylene dioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCOC(=O)CCCCCCC\C=C/CCCCCCCC NKSOSPOXQKNIKJ-CLFAGFIQSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000000976 ink Substances 0.000 description 9
- 239000003973 paint Substances 0.000 description 6
- 150000003014 phosphoric acid esters Chemical group 0.000 description 6
- 239000000049 pigment Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- -1 phosphate ester Chemical class 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229960002317 succinimide Drugs 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 150000005691 triesters Chemical class 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/324—Inkjet printing inks characterised by colouring agents containing carbon black
- C09D11/326—Inkjet printing inks characterised by colouring agents containing carbon black characterised by the pigment dispersant
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
Description
본 발명은 분산제 제조 방법에 관한 것으로서, 특히, 잉크 또는 페인트 등의 물질에 사용되는 분산제로서 단일직쇄분산제에 비해 다수의 직쇄 분산제를 갖는 인산에스테르를 이용하여 분산 효과를 향상시킬 수 있는 분산제를 제조하는 방법에 관한 것이다. The present invention relates to a method for preparing a dispersant, and more particularly, to prepare a dispersant capable of improving the dispersing effect by using a phosphate ester having a plurality of linear dispersants compared to a single linear dispersant as a dispersant used in materials such as ink or paint. It's about how.
분산제는 유용성 (oil-soluble type) 계면활성제 형태의 구조를 갖고 있어 극성 퇴적물을 연료유 중에 분산시키고 엔진 내부의 노즐 등에 부착된 물질들을 용해하여 분산시키는 역할을 한다. 분산제로 사용가능한 것은 아미드, 아민, 폴리부텐숙신이미드, 폴리올레핀 아민류, 폴리에테르 아민 등이 있다. The dispersant has a structure in the form of an oil-soluble type surfactant, and serves to disperse polar deposits in fuel oil and dissolve and disperse materials attached to nozzles inside the engine. Dispersants that can be used include amides, amines, polybutene succinimide, polyolefin amines, and polyether amines.
분산제를 용제에 희석시킨 상태로 사용하고 있으며, 이들 화합물의 약 300 ppm 정도를 경유에 첨가하여 사용하고 있다.Dispersants are used diluted in solvents, and about 300 ppm of these compounds are added to light oil.
한편, 한국 등록특허 제10-020234호에는 잉크젯 프린터용 승화형 잉크 및 종이에 인쇄한 후, 열전사 시키는 인쇄방법이 개시되어 있으나, 전사지가 아닌 일반용지에 인쇄하여 전사할 수 있고 다양한 소재에 적용할 수 있다는 장점이 있으나, 카본 농도가 낮아 인쇄성이 나쁘고 분산성이 낮아 고체입자가 쉽게 침전되며 저장안정성에 문제점이 있을 뿐만 아니라 색상 구현성이 좋지 않다는 단점이 있다.On the other hand, Korean Patent Registration No. 10-020234 discloses a sublimation ink for an inkjet printer and a printing method of thermal transfer after printing on paper, but it can be printed on plain paper rather than transfer paper and transferred and applied to various materials However, there are disadvantages in that the carbon concentration is low and the printability is poor and the dispersibility is low, so that solid particles are easily precipitated, and there is a problem in storage stability as well as poor color implementation.
이에 인쇄성이 좋고, 분산성 및 저장안전성이 우수한 잉크젯 프린터용 잉크 조성물 특히, 이미지를 잉크젯 프린터로 일반용지에 인쇄한 후, 열을 가하여 섬유나 도자기 등에 이미지를 전사할 수 있는 전사잉크 조성물이 필요한 실정이다.Accordingly, an ink composition for an inkjet printer having good printability, dispersibility and storage stability, in particular, a transfer ink composition capable of transferring an image to textiles or ceramics by applying heat after printing an image on plain paper with an inkjet printer is required. The situation is.
이에 본 발명은 잉크 및 페인트 등에 사용되는 분산제로서, 연료유, 오일, 잉크, 페인트, 코팅제등에 포함되는 다양한 종류의 카본, 안료 등을 효과적으로 분산하는 분산제를 제공하는 것에 그 목적이 있다.Accordingly, an object of the present invention is to provide a dispersant that effectively disperses various types of carbon, pigments, etc. included in fuel oil, oil, ink, paint, coating agent, etc. as a dispersant used in ink and paint.
실시예의 분산제 제조 방법은, 계면활성제로서 트리데실 알코올 에테르(TDE, TRIDECYL ALCOHOL ETHER)를 반응기에 넣고, 상기 반응기를 50℃까지 승온시키는 단계와, 상기 TDE와 반응시키기 위한 인산을 기설정된 양만큼 투입하면서, 반응기의 온도를 60±3℃까지 상승시키는 단계와, 상기 인산을 기설정된 양만큼 다시 투입하고, 상기 반응기의 교반 및 색상 관찰을 수행하는 단계로서, 기설정된 양의 인산을 모두 투입하는 때까지 반복하는 단계와, 기설정된 온도까지 상승시킨 후, 숙성시키는 단계와, 상기의 숙성시키는 단계 이후에, 유화제로서 폴리에틸렌글리콜 디올리에이트(PEG dioleate)를 기설정된 양만큼 투입하는 단계를 포함한다. The dispersant manufacturing method of the embodiment includes the step of putting tridecyl alcohol ether (TDE, TRIDECYL ALCOHOL ETHER) as a surfactant into a reactor, raising the temperature of the reactor to 50 ° C, and adding a predetermined amount of phosphoric acid to react with the TDE while raising the temperature of the reactor to 60 ± 3 ° C, re-injecting the phosphoric acid by a predetermined amount, and performing stirring and color observation of the reactor, when all the phosphoric acid in the predetermined amount is added It includes the step of repeating up to, raising to a predetermined temperature, then aging, and after the aging, adding polyethylene glycol dioleate (PEG dioleate) as an emulsifier in a predetermined amount.
그리고, 상기 TDE, 인산 및 폴리에틸렌글리콜 디올리에이트의 함량 비율은, 2,800~32,000kg 범위의 TDE와, 200~240kg 범위의 인산과, 800kg의 폴리에틸렌글리콜 디올리에이트를 사용하는 것을 특징으로 한다. In addition, the content ratio of the TDE, phosphoric acid and polyethylene glycol dioleate is characterized by using TDE in the range of 2,800 to 32,000 kg, phosphoric acid in the range of 200 to 240 kg, and polyethylene glycol dioleate in the range of 800 kg.
그리고, 상기 숙성시키는 단계는 상기 반응기의 온도를 70℃로 유지한 상태에서 수행되는 것을 특징으로 한다. In addition, the aging step is characterized in that it is performed while maintaining the temperature of the reactor at 70 ℃.
그리고, 상기 유화제를 투입한 다음에는, 상기 반응기의 온도를 40℃이하로 냉각하는 과정을 더 수행하는 것을 특징으로 한다. In addition, after the emulsifier is added, a process of cooling the temperature of the reactor to 40° C. or less is further performed.
제안되는 본 발명의 분산제 제조 방법에 의해서, 단일직쇄분산제를 분산 반응을 일으키는 가지가 많은 분산제로 유도반응시킴으로써, 분산 효과를 더욱 높일 수 있는 장점이 있다. According to the proposed method for preparing a dispersant of the present invention, a dispersing effect can be further enhanced by inducing a reaction of a single linear dispersing agent with a dispersing agent having many branches causing a dispersing reaction.
도 1은 본 발명에 따른 분산제 제조 방법을 설명하기 위한 흐름도이다.
도 2는 본 발명에 따른 분산제 제조 방법에서 알코올과 인산의 반응으로 발생되는 인산에스테르 구조를 보여주는 도면이다.
도 3은 본 실시예에 따라 제조되는 인산에스테르계 분산제의 구조와 기존의 다른 분산제 구조를 개략적으로 비교하기 위한 도면이다.
도 4 내지 도 6은 해당 실험을 통해 측정한 점도의 값을 보여주는 사진이다. 1 is a flow chart for explaining a method for preparing a dispersant according to the present invention.
2 is a view showing the phosphoric acid ester structure generated by the reaction of alcohol and phosphoric acid in the method for preparing a dispersant according to the present invention.
Figure 3 is a diagram for schematic comparison between the structure of a phosphoric acid ester-based dispersant prepared according to this embodiment and the structure of other existing dispersants.
4 to 6 are photographs showing the values of viscosity measured through the experiment.
이하, 첨부된 도면을 참조하여 본 명세서에 개시된 실시 예를 상세히 설명하되, 도면 부호에 관계없이 동일하거나 유사한 구성요소는 동일한 참조 번호를 부여하고 이에 대한 중복되는 설명은 생략하기로 한다. 이하의 설명에서 사용되는 구성요소에 대한 접미사 "모듈" 및 "부"는 명세서 작성의 용이함만이 고려되어 부여되거나 혼용되는 것으로서, 그 자체로 서로 구별되는 의미 또는 역할을 갖는 것은 아니다. 또한, 본 명세서에 개시된 실시 예를 설명함에 있어서 관련된 공지 기술에 대한 구체적인 설명이 본 명세서에 개시된 실시 예의 요지를 흐릴 수 있다고 판단되는 경우 그 상세한 설명을 생략한다. 또한, 첨부된 도면은 본 명세서에 개시된 실시 예를 쉽게 이해할 수 있도록 하기 위한 것일 뿐, 첨부된 도면에 의해 본 명세서에 개시된 기술적 사상이 제한되지 않으며, 본 발명의 사상 및 기술 범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. Hereinafter, the embodiments disclosed in this specification will be described in detail with reference to the accompanying drawings, but the same or similar elements are given the same reference numerals regardless of reference numerals, and redundant description thereof will be omitted. The suffixes "module" and "unit" for components used in the following description are given or used together in consideration of ease of writing the specification, and do not have meanings or roles that are distinct from each other by themselves. In addition, in describing the embodiments disclosed in this specification, if it is determined that a detailed description of a related known technology may obscure the gist of the embodiment disclosed in this specification, the detailed description thereof will be omitted. In addition, the accompanying drawings are only for easy understanding of the embodiments disclosed in this specification, the technical idea disclosed in this specification is not limited by the accompanying drawings, and all changes included in the spirit and technical scope of the present invention , it should be understood to include equivalents or substitutes.
어떤 구성요소가 다른 구성요소에 "연결되어" 있다거나 "접속되어" 있다고 언급된 때에는, 그 다른 구성요소에 직접적으로 연결되어 있거나 또는 접속되어 있을 수도 있지만, 중간에 다른 구성요소가 존재할 수도 있다고 이해되어야 할 것이다. 반면에, 어떤 구성요소가 다른 구성요소에 "직접 연결되어" 있다거나 "직접 접속되어" 있다고 언급된 때에는, 중간에 다른 구성요소가 존재하지 않는 것으로 이해되어야 할 것이다.It is understood that when an element is referred to as being "connected" or "connected" to another element, it may be directly connected or connected to the other element, but other elements may exist in the middle. It should be. On the other hand, when an element is referred to as “directly connected” or “directly connected” to another element, it should be understood that no other element exists in the middle.
도 1은 본 발명에 따른 분산제 제조 방법을 설명하기 위한 흐름도이다. 1 is a flow chart for explaining a method for preparing a dispersant according to the present invention.
페인트 잉크에 사용되는 분산제를 제조하기 위하여 계면활성제로서 트리데실 알코올 에테르(TDE, TRIDECYL ALCOHOL ETHER)와, 상기 계면활성제와의 반응을 통해 인산(Phosphorus pentoxide, 오산화인) 및 유화제로서 폴리에틸렌글리콜-n 디올리에이트(PEG-n dioleate)를 사용한다. In order to prepare a dispersant used in paint ink, tridecyl alcohol ether (TDE, TRIDECYL ALCOHOL ETHER) as a surfactant and phosphoric acid (Phosphorus pentoxide, phosphorus pentoxide) through reaction with the surfactant and polyethylene glycol-ndi as an emulsifier Oleate (PEG-n dioleate) is used.
본 발명에서는 TDA가 가공된 TDE, 인산 및 폴리에틸렌글리콜 디올리에이트의 함량(중량) 비율은, 2,800~32,000kg 범위의 TDE와, 200~240kg 범위의 인산과, 800kg의 폴리에틸렌글리콜-n 디올리에이트를 사용한다. In the present invention, the content (weight) ratio of TDE processed by TDA, phosphoric acid and polyethylene glycol dioleate is TDE in the range of 2,800 to 32,000 kg, phosphoric acid in the range of 200 to 240 kg, and polyethylene glycol-n dioleate in the range of 800 kg Use
먼저, 반응기에 원료인 TDE를 투입(S110)하고, 반응기의 온도를 50℃까지 상승시킨다(S120). 여기서, 반응기의 내부의 온도를 50℃로 상승시키는 이유는 후속되는 인산과의 반응이 시작되는 온도이기 때문이다. First, TDE as a raw material is introduced into the reactor (S110), and the temperature of the reactor is raised to 50°C (S120). Here, the reason why the temperature inside the reactor is raised to 50° C. is that it is the temperature at which the subsequent reaction with phosphoric acid starts.
그 다음, 기설정된 양, 예를 들어, 2~3kg씩 인산을 상기 반응기에 투입하고(S130), 반응기의 온도를 기준온도인 60±3℃까지 제어하며, 상기 반응기 온도가 기준온도인 60℃±3℃를 유지(S140)하면서 인산을 2~3kg씩 투입(S150)하며, 이것은 60℃ 부근에서 가장 활발한 인산 반응이 일어나기 때문이다. Then, a predetermined amount, for example, 2 to 3 kg of phosphoric acid is introduced into the reactor (S130), and the temperature of the reactor is controlled to a reference temperature of 60 ± 3 ° C, and the reactor temperature is a reference temperature of 60 ° C. While maintaining ±3 ° C (S140), 2 to 3 kg of phosphoric acid is added (S150), because the most active phosphoric acid reaction occurs around 60 ° C.
2~3kg을 초과하는 인산을 투입하는 경우에는 과도한 반응으로 인해 높은 열이 발생하여 모노에스테르, 디에스테르, 및 트리에스테르 혼합물이 생성되기 어렵기 때문이다. This is because when phosphoric acid in excess of 2 to 3 kg is added, high heat is generated due to excessive reaction, making it difficult to produce monoester, diester, and triester mixtures.
이때, 알코올과 인산과의 반응은 도 2에 도시된 바와 같이 TDE와 인산의 화학 반응을 통해, 3가지 종류의 인산에스테르가 형성된다. 3ROH(고급알콜)과 P2O5 (무수인산)의 반응 비율은, 대략 인산 : 알코올 = 1:3의 비율로 반응을 시작한다. 일반적인 직쇄분산제에 비하여 인산에스테르는 복수개의 직쇄분산제를 가지고 있는 구조로서, 일반 분산제 1개가 안료쪽으로 배향을 해서 분산효과를 주는 것에 비하여, 3개의 직쇄로 인한 입체장애효과로 안료를 충분히 탈응집시켜 2~3배의 안정화 효과를 갖게 된다. At this time, the reaction between alcohol and phosphoric acid is a chemical reaction between TDE and phosphoric acid, as shown in FIG. 2, to form three types of phosphoric acid esters. The reaction ratio between 3ROH (higher alcohol) and P 2 O 5 (anhydrous phosphoric acid) starts at a ratio of approximately phosphoric acid : alcohol = 1:3. Compared to general linear dispersants, phosphoric acid ester has a structure that has a plurality of linear dispersants. Compared to one general dispersant that is oriented toward the pigment to give a dispersing effect, the steric hindrance effect caused by three linear chains sufficiently deagglomerates the pigment, resulting in 2 It has a stabilizing effect of ~3 times.
그리고, 다시 반응기를 교반시키면서 인산과 TDE의 반응 후 투명하게 되는지 여부를 관찰하고, 반응이 완료되었음을 알 수 있는 투명도를 갖는 경우에 상기 단계 S150 및 S160을 반복하여 수행함으로써, 200~240kg 범위의 인산, 예를 들면, 220kg의 인산을 모두 3,000kg의 TDE에 반응시킨다. Then, while stirring the reactor again, observe whether or not it becomes transparent after the reaction of phosphoric acid and TDE, and when it has a transparency that indicates that the reaction is complete, by repeating the above steps S150 and S160, phosphoric acid in the range of 200 to 240 kg , for example, 220 kg of phosphoric acid are all reacted with 3,000 kg of TDE.
본 발명의 실시예에 따라 정해진 인산의 양을 모두 반응시킨 다음에는, 반응기의 온도를 70℃로 유지하면서 2시간의 숙성과정을 수행한다(S180). 이때의 숙석 과정은 반응물 완성도(반응률)가 100%에 가깝도록 하기 위하여 앞선 반응온도인 60℃ 보다 높은 온도인 70℃까지 서서히 상승 및 지속시키면서 미반응물질이 줄어들도록 하는 과정이다. After reacting all the amount of phosphoric acid determined according to the embodiment of the present invention, a 2-hour aging process is performed while maintaining the temperature of the reactor at 70 ° C (S180). At this time, the sintering process is a process in which unreacted substances are reduced while gradually raising and continuing to a temperature higher than the previous reaction temperature of 60 ° C. to 70 ° C. so that the completeness (reaction rate) of the reactants is close to 100%.
그 다음, 산가 100~120의 범위를 갖는 확인(S190)하고, 유화제로서 폴리에틸렌글리콜 디올리에이트(PEG dioleate) 800kg을 투입(S200)한다. 폴리에틸렌글리콜 디올리에이트(PEG dioleate)는 계면활성도가 높은 물질로서, 최종적으로 제조되는 분산제의 효과를 크게 높일 수 있다. 이에 대해서는, 첨부되는 도면과 함께 실험 결과를 설명하여 본다. 한편, PEG 투입 후에는 반응기의 가열을 종료한 뒤 40℃이하로 냉각한 다음 배출(S210)하여 최종적인 분산제 제조 과정을 종료한다. Then, it is confirmed that it has an acid value in the range of 100 to 120 (S190), and 800 kg of polyethylene glycol dioleate (PEG dioleate) is added as an emulsifier (S200). Polyethylene glycol dioleate (PEG dioleate) is a material with high surface activity, and can greatly increase the effect of the finally prepared dispersant. In this regard, the experimental results will be described together with the accompanying drawings. On the other hand, after PEG is added, the heating of the reactor is finished, cooled to 40 ° C. or less, and then discharged (S210) to complete the final dispersant preparation process.
도 3은 본 실시예에 따라 제조되는 인산에스테르계 분산제의 구조와 기존의 다른 분산제 구조를 개략적으로 비교하기 위한 도면이다. Figure 3 is a diagram for schematic comparison between the structure of a phosphoric acid ester-based dispersant prepared according to this embodiment and the structure of other existing dispersants.
즉, 본 실시예에 따라 TDE와 인산의 화학 반응을 통해, 안료친화기 가지수가 많은 인산에스테르 분산제의 경우, 보다 효과적으로 분산제의 역할을 수행할 수 있다. That is, in the case of a phosphoric acid ester dispersant having a large number of pigment affinity groups through a chemical reaction between TDE and phosphoric acid according to the present embodiment, it can more effectively serve as a dispersant.
아래의 표 1은 본 실시예에 따라 제조된 분산제를 첨가한 경우, 분산제를 첨가하지 않은 경우 및 시중에 판매되는 일반분산제를 첨가한 경우에 페인트 잉크의 점도(분산력)를 확인한 실험데이터이다. Table 1 below shows experimental data confirming the viscosity (dispersion power) of the paint ink when the dispersant prepared according to this example was added, when the dispersant was not added, and when a commercially available general dispersant was added.
안료인 탄산칼슘과, 가소제를 75:25로 배합하고, 추가로 함량비 1에 해당하는 무게만큼 분산제를 넣은 경우이고, 도 4 내지 도 6은 해당 실험을 통해 측정한 점도의 값을 보여주는 사진이다. When calcium carbonate, which is a pigment, and a plasticizer are mixed at a ratio of 75:25, and a dispersant is added by weight corresponding to the content ratio 1, FIGS. 4 to 6 are photographs showing the viscosity values measured through the experiment .
실험한 결과, 본 실시예의 경우, 강한 산성을 갖는 분산제로서, 일반적인 분산제를 사용한 경우보다 점도가 4% 수준으로 낮출 수 있으며, 이는 분산제로서 페인트 잉크가 굳는 현상을 현저히 떨어뜨릴 수 있음을 알 수 있다. As a result of the experiment, in the case of this embodiment, as a dispersant having strong acidity, the viscosity can be lowered to a level of 4% compared to the case of using a general dispersant, which can significantly reduce the hardening of paint ink as a dispersant. .
Claims (4)
상기 인산을 기설정된 양만큼 다시 투입하고, 상기 반응기의 교반 및 색상 관찰을 수행하는 단계로서, 기설정된 양의 인산을 모두 투입하는 때까지 반복하는 단계와,
기설정된 온도까지 상승시킨 후, 숙성시키는 단계와,
상기의 숙성시키는 단계 이후에, 유화제로서 폴리에틸렌글리콜 디올리에이트(PEG dioleate)를 기설정된 양만큼 투입하는 단계를 포함하는 분산제 제조 방법. Raising the temperature of the reactor to 60 ± 3 ° C. while adding a predetermined amount of tridecyl alcohol ether (TDE, TRIDECYL ALCOHOL ETHER) processed as a surfactant and phosphoric acid to react with the TDE;
Re-injecting the phosphoric acid in a predetermined amount and performing stirring and color observation of the reactor, repeating until all the phosphoric acid in the predetermined amount is added;
After raising to a predetermined temperature, aging step;
After the aging step, a dispersant manufacturing method comprising the step of introducing a predetermined amount of polyethylene glycol dioleate (PEG dioleate) as an emulsifier.
상기 TDE, 인산 및 폴리에틸렌글리콜 디올리에이트의 함량 비율은, 2,800~32,000kg 범위의 TDE와, 200~240kg 범위의 인산과, 800kg의 폴리에틸렌글리콜 디올리에이트를 사용하는 것을 특징으로 하는 분산제 제조 방법. According to claim 1,
The content ratio of TDE, phosphoric acid and polyethylene glycol dioleate is a dispersant manufacturing method, characterized in that using TDE in the range of 2,800 to 32,000 kg, phosphoric acid in the range of 200 to 240 kg, and polyethylene glycol dioleate in the range of 800 kg.
상기 숙성시키는 단계는 상기 반응기의 온도를 70℃로 유지한 상태에서 수행되는 것을 특징으로 하는 분산제 제조 방법. According to claim 2,
The aging step is a dispersant manufacturing method, characterized in that carried out in a state where the temperature of the reactor is maintained at 70 ℃.
상기 유화제를 투입한 다음에는, 상기 반응기의 온도를 40℃이하로 냉각하는 과정을 더 수행하는 것을 특징으로 하는 분산제 제조 방법.
According to claim 3,
After the emulsifier is added, a dispersant manufacturing method characterized in that further performing a process of cooling the temperature of the reactor to 40 ℃ or less.
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| US5464874A (en) * | 1991-04-30 | 1995-11-07 | Huels Aktiengesellschaft | Aqueous surfactant compositions of elevated viscosity |
| KR100771786B1 (en) * | 2003-04-01 | 2007-10-30 | 악조 노벨 엔.브이. | Dispersion |
| KR101127959B1 (en) * | 2011-11-18 | 2012-04-04 | (재)한국섬유소재연구소 | Dispersing agent and manufacturing method thereof |
| US20200172831A1 (en) * | 2018-11-30 | 2020-06-04 | Ecolab Usa Inc. | Surfactant compositions and use thereof |
| JP2021030223A (en) * | 2019-08-19 | 2021-03-01 | 三洋化成工業株式会社 | Dispersant for inorganic filler |
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| US5464874A (en) * | 1991-04-30 | 1995-11-07 | Huels Aktiengesellschaft | Aqueous surfactant compositions of elevated viscosity |
| KR100771786B1 (en) * | 2003-04-01 | 2007-10-30 | 악조 노벨 엔.브이. | Dispersion |
| KR101127959B1 (en) * | 2011-11-18 | 2012-04-04 | (재)한국섬유소재연구소 | Dispersing agent and manufacturing method thereof |
| US20200172831A1 (en) * | 2018-11-30 | 2020-06-04 | Ecolab Usa Inc. | Surfactant compositions and use thereof |
| JP2021030223A (en) * | 2019-08-19 | 2021-03-01 | 三洋化成工業株式会社 | Dispersant for inorganic filler |
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