KR910006620B1 - Process for making calcium grutamic acid - Google Patents
Process for making calcium grutamic acid Download PDFInfo
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- KR910006620B1 KR910006620B1 KR1019890019883A KR890019883A KR910006620B1 KR 910006620 B1 KR910006620 B1 KR 910006620B1 KR 1019890019883 A KR1019890019883 A KR 1019890019883A KR 890019883 A KR890019883 A KR 890019883A KR 910006620 B1 KR910006620 B1 KR 910006620B1
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- calcium
- glutamic acid
- glutamate
- acid
- grutamic
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/40—Table salts; Dietetic salt substitutes
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
Description
본 발명은 당질을 주원료로 사용하여 미생물 발효에 의하여 얻어진 L-글루타민산 발효액으로부터 공업적으로 제조공정이 간단하고 수율이 우수한 글루타민산 칼슘염을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing calcium glutamate salt having a simple production process and excellent yield from L-glutamic acid fermentation broth obtained by microbial fermentation using sugar as a main raw material.
일반적으로 식품첨가물로 사용되는 글루타민산 염으로는 글루타민산 나트륨, 글루타민산 칼륨, 글루타민산 암모늄 및 글루타민산 칼슘염등이 있으나, 이들중 정미력은 글루타민산 나트륨이 가장 우수하지만 이를 과잉으로 섭취할 경우에는 체내에서 유리되는 나트륨 이온에 의한 혈압상승이 우려되는 문제점이 있음이 학계에 보고된 바 있다.In general, glutamate salts used as food additives include sodium glutamate, potassium glutamate, ammonium glutamate, and calcium glutamate. Among them, the glutamate has the best sodium glutamate, but when it is ingested in excess, sodium is liberated in the body. It has been reported in the academic community that there is a concern that the increase in blood pressure caused by ions.
따라서 본 발명자들은 이러한 글루타민산 나트륨염의 단점을 개선키 위하여 근래에 각광을 받고 있는 인체작용에 있어서 상승효과가 있는 글루타민산 칼슘염의 새로운 제조방법을 개발하여 본 발명을 완성하였다.Therefore, the present inventors have completed the present invention by developing a new method for preparing calcium glutamate, which has a synergistic effect in the human body, which has recently been in the spotlight in order to improve the disadvantage of sodium glutamate.
즉, 본 발명에 의한 글루타민산 칼슘염의 제조방법은 글루타민산 나트륨의 제조방법과 같은 글루타민산을 분리하고 회수하는 제1공정과 분리된 글루타민산을 칼슘염으로 제조하는 제2공정으로 구성된 것으로, 이를 좀더 구체화하면, 글루타민산을 분리, 회수하는 공정인 제1공정에서는 글루타민산 발효액을 진한 황산으로 pH 3.2까지 중화하여 결정용액으로 제조한 다음, 이 용액을 냉각하고 정석 분리한 결정을 2-3단계의 세척공정을 거쳐 순도가 좋은 글루타민산으로 제조하고 ; 제2공정에서는 고순도의 글루타민산에 60℃의 가온수를 가하여 용액의 농도를 40-55%로 조정한 후 가온수에 슬러리인 수산화칼슘을 글루타민산 당량비만큼 첨가하여 완전히 용애하고 최종 pH와 농도(최적 pH는 6-7, 농도는 40-55%)를 확인한 다음, 후속공정으로 이송시켜 중화한 글루타민산 칼슘용액에 활성탄을 글루타민산 대비 2%(wt/wt)첨가하여 60℃에서 2시간동안 탈색한 다음, 여과기를 이용하여 색소가 흡착된 폐 활성탄과 탈색여액을 분리하는 공정이다. 이 공정에서 유의하여야 할 것은 여과시에 칼슘염이 석출될 위험성이 있으므로 분리가 완료될 때가지 60℃의 온도로 계속 유지시켜야 하는 점이다.That is, the method for preparing calcium glutamate salt according to the present invention comprises a first step of separating and recovering glutamic acid, such as a method for producing sodium glutamate, and a second step of preparing the separated glutamic acid as a calcium salt. In the first step, which is a process of separating and recovering glutamic acid, the glutamic acid fermentation broth is neutralized with concentrated sulfuric acid to pH 3.2 to prepare a crystal solution.The solution is cooled and the crystals separated by crystallization are purified through 2-3 steps of purity. Is prepared with good glutamic acid; In the second step, high-purity glutamic acid is added to hot water at 60 ° C to adjust the concentration of the solution to 40-55%, and then calcium hydroxide as slurry is added to the warm water by the equivalent ratio of glutamic acid to completely melt the final pH and concentration (the optimal pH is 6-7, the concentration is 40-55%), and then transferred to the subsequent process to add 2% (wt / wt) of activated carbon to the neutralized calcium glutamate solution and decolorize at 60 ° C for 2 hours, and then It is a process of separating the waste activated carbon and the decoloration filtrate adsorbed by the pigment. It should be noted that in this process, calcium salts are precipitated during filtration, so they must be maintained at a temperature of 60 ° C. until separation is completed.
일반적으로 칼슘염은 농축 또는 유기용매를 첨가하지 않아도 냉각, 정석법에 의하여 용이한 결정을 얻을 수 있기 때문에 제조공정상 설비가 단순한 이점이 있다. 다음에는 탈색 분리된 여액을 10℃까지 냉각하고 일정량의 종정(Seed)를 첨가하여 결정 크기의 균일화 및 칼슘염의 생성을 촉진시킨다. 10℃의 온도를 계속 유지시켜주면서 10-50시간 정석하여 입자 숙성을 행한 다음, 고속원심분리기 또는 탈수분리기를 이용하여 분리한다. 분리된 결정은 고순도의 제품으로 분말결정과 크리스탈입자로 구성되어 있었으며 칼핏셔 수분측정결과, 2.3-4H2O 분자를 갖고 있었으며 본 발명에 의한 글루타민산 칼슘염과 글루타민산 나트륨염과의 맛 선호도 실험결과는 다음의 표 1에 기재하였다.In general, since calcium salts can be easily obtained by cooling or crystallization without the addition of concentrated or organic solvents, the facilities have simple advantages in the manufacturing process. The decolorized separated filtrate is then cooled to 10 ° C. and a certain amount of seed is added to promote homogenization of crystal size and formation of calcium salt. While maintaining the temperature of 10 ℃ is crystallized for 10 to 50 hours to carry out the particles and then separated using a high-speed centrifuge or a dehydration separator. The separated crystal was a high-purity product composed of powder crystals and crystal grains. As a result of Karl Fischer's moisture measurement, it had 2.3-4H 2 O molecules, and the taste preference test result of calcium glutamate and sodium glutamate salt according to the present invention It is shown in Table 1 below.
[표 1]TABLE 1
상기 표의 기재와 같이 맛 선호도를 비교한 결과, 정미력면에서 글루타민산 칼슘염은 글루타민산 나트륨염과 대등하였음을 확인할 수 있었다.As a result of comparing the taste preference as described in the table, it was confirmed that calcium glutamate was equivalent to sodium glutamate in terms of taste.
다음의 실시예에서 본 발명을 좀더 구체적으로 설명한다.The present invention is explained in more detail in the following examples.
[실시예 1]Example 1
글루타민산 2Kg에 60℃의 가온수를 가하여 40% 글루타민산 용액으로 한 후, 수산화칼슘을 400g 첨가하여 pH를 6.3으로 조절하고, 이 용액에 활성탄 40g을 가한 다음, 60℃에서 2시간 탈색하고 분리한 분리여액을 15℃까지 냉각한 후 칼슘화합물의 종정 5g(wt/wt)을 가하고 10시간 동안 정석한 다음, 분리하므로써 고순도의 글루타민산 칼슘염 1.44Kg을 얻었다. 칼핏셔 수분측정결과 4H2O 물분자를 함유하고 있는 것으로 확인되었다.After adding hot water at 60 ° C to 40% glutamic acid solution to 2 Kg of glutamic acid, 400 g of calcium hydroxide was added to adjust the pH to 6.3. 40 g of activated carbon was added to the solution, followed by decolorization at 60 ° C. for 2 hours. After cooling to 15 ° C 5g (wt / wt) of the calcium compound was added and crystallized for 10 hours, and separated to obtain 1.44Kg of high purity calcium glutamate salt. Karl Fischer moisture determination revealed that it contained 4H 2 O water molecules.
[실시예 2]Example 2
글루타민산 1Kg에 60℃의 가온수를 기하여 55% 용액으로 조정한 다음, 수산화칼슘 175g을 첨가하여 pH를 7.0으로 조절한 후 이 용액에 활성탄을 가하여 60℃에서 2시간동안 탈색하여 용액중의 색소를 제거한 다음, 10℃로 냉각하여 50시간 정석하고 고속원심분리기로 분리하여 고순도의 글루타민산 칼슘염 0.72Kg을 얻었다. 칼핏셔 수분측정결과 3.0H2O 물분자를 함유하고 있는 것으로 확인되었다.Adjust the pH to 7.0 by adding hot water at 60 ℃ to 1 Kg of glutamic acid, adjust pH to 7.0 by adding 175g of calcium hydroxide, and decolorize at 60 ℃ for 2 hours to remove pigment in solution. Next, the mixture was cooled to 10 ° C., crystallized for 50 hours, and separated by a high-speed centrifuge to obtain 0.72 Kg of calcium glutamate of high purity. Karl Fischer moisture determination revealed that it contained 3.0H 2 O water molecule.
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KR1019890019883A KR910006620B1 (en) | 1989-12-28 | 1989-12-28 | Process for making calcium grutamic acid |
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KR1019890019883A KR910006620B1 (en) | 1989-12-28 | 1989-12-28 | Process for making calcium grutamic acid |
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